NEW EDITION

• Che1 nistry

Chemistry Laboratory Skills

G eorge Facer
>- clear revision guidance
>- examiner advice
PHILIP ALLAN
- sample tasks
 STUDENT UNIT GUIDE

NEW EDITION

• ..
Ed excel AS/A2 Chernist:ry
Unit:s 3 and 6
Chernist:ry Laboratory Sl<ills

Geor·ge Facer·

PHILIP ALLAN
 PhtHp Allan. an tmprtnt or HOdder Educauon. an Hacheue UK company, Mackel Place, Oedd.tngton,
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 Contents
Get·ttna the mos t f"ro en this book ........... . .. . . . ...... •............................................. .... •...... •......................... 4
About this book .......................... . . ..... •...... •.... •...... •......................... 5

C o n te n t Guida n ce
Unit 3 ...... . ...... ...... ..... .. .. ................................................................................... •...... . .... ..... .......... . .. .... ..... .. ... . 8
Activity B: Qualttallve obsea·vatiOa1 ... ... ... ......... ....... .......... .. ... .. ............... . ... ... . .... ... ... . .......... ....... ................ 8
Activity C: Quantitative m easu re anent ...................................................................................................... 17
Act1vity 0 : Preparatton ................................................................................................................................27
Unit 6 ..........................................................................................................................................................33
Activity B : Quallt~ U ve obse 1·vat1on ............. . .... . ...... . ........ . . ..... .. .... ...... .. ............... ... .... 33
Activ ity C: Quantitative n"''easurement . . ............................................... ....................... 44
Activ ity D : Propc:u·auon .............. . ..... ................................. 51

Questions & Ans w e r s

T est q uestlons with a -nswers ....................................... . . . .... . .... . ...... . ....................... 67

• T est question 1 ......... .

Test question 2 ......... .
Tes t quesuon 3 ......... .
. . ...... . ....................... 58
. . ...... . ...................... 59 ..
.... .. ...................... . .... .. . .... . ...... . ......... . ............. 62
, -est question 4 ........... . .............................................................................................................................6~
' J' est <:1uestton ~ .......................................................... . ..... ................................... ..... ..... .. ..... . ....................... 67
1'est quest ton 6 ............... ..... ... .... ............................... .. ... .................................. ....... ... .. ..... .. .. ......................68

Knowl eds;te c h eck answers ....................................................................................................................70

I nd ex ........................................................................................................................................................... 76
P eriodic tabl e .............................................. .... . ..... ... .. .. ......................................... ... .. ...... . ....................... 79
 Getting the most "from this book

E x ••••i u ~ r Li p~
Ad....;co (ror,-, tho oxnrornincn- o n lcoy poin-ts in t h ea Knowl edge c h ~ck
"text t:o help you learn and recall uni t: content:. Rapid-fire question • throuah ovt the C o n tent
tsvoid p i t f .:tlls , and polish your ex"*M technique in Guidance section 'to check you r understand i n~.
ol'"'dfar to boost your S~Jddo .

Knowled e c h eck answer· s Su1"1""1mariea

• i;:.:ach cor e topic is roundGtd off by ::..
1 Tu,..... to the b:.ck or 'the book ror 'the Knowledae t>ul let.- llst summary for quicK- checK
c:heck .ans\llo'ers. refEu·ence or what you need to know.

• ..
Q uestions & Answers

Exa •n - s tylo questio n s ------J_.......-.._.....__ ...__ ...... _____ __ _

I"'" .., _ _,

·-
._ ,

Exa •n•ne .- cotnn'len ts

o n the questio n s
Tips on what you
need to do to gatn f"all -----,..•--c.
(10>1_

..
_
...... ..._....._.......... ________ .. ·-
.. ::.:..~::::::::.:::-::..":"-":.:=.-:.:.~::=--"".!:_~...""·"'-" ...
....... - . . . . . - -... _~

.....____ .... -· ·-
_.._,..,.. __ . . ..·---
::.::..."":.~..::::..=·=-.·::::.-::::_"=:--
n'\arks, tndtcated by the
leon \.::tt. ------·----·- ,__, ,.,. "'',.._..,,_.,...__,

sampl e stu d e nt T-.---·--

----· ..--..·---'
,.._._,..,.,_ _ ••·--..- -,- c,., ___
n n swers
Prac u se the Questtons.
then took a t the s tudent
=---·"'----.
~==-....-::~~o:.::.--::::-:::::::..<:.:.c:::.'!.,

•t ~;::...'"';:.;:;-.::r...::::-:-.:=::::==.:'--.-
X:::.;:;-.:..-.(;.';:;;:;::;-"'--·-- --
__ ..

- -........
answers that follow
each Questton .
---·-·----
4 Ede><:Cel A S/A2 ChEHY'Ii stry
 About: t:his book
This g u ldo I s o n e of tho series coveri n g tho Edcxcol s pcclflcnllo n f or AS nnd A2
c h e mistry. 1t o ffe r s adv ice ro r effectiv e p r epa r a tto n for t h e unit 3 L-Bbor atory S kflls
Jnte cna l assessment and the unit 6 Laborator-y Skills internal assessmenl.
Each section fnch.t dcs u. number o f knowledge c h ecks, son'lo of w hich require you t o
write dow n the observatio n s that would be m ade a n d t h e n a n swe•· som e follow- up
quesuo.,s. or to h and le data rrom quarultauve measuremen ts Or" preparations. T h e
answer s to these ca n be found o n pngcs 7 0~75. Ench .,. tnrorms you of a scoring p o int.

rn each o f the Un it 3 a nd Unit 6 pa r ts o f t h e Question s &. Answers sectio n there a r e

two mock A c ttvtty Band one Acllvlty c ptactlcal experiment s (Ca lled test quesuons)
that you cn n try, so l o ng as they aro s upervised and havo been rt.sk- nssessod by a
c h e mist-r y t .each er. Answers are pro vided after each test question.
Pour a•sunct skills are requtrea In advanced l evel pracucal c h e•nLst ry.

A G e n e r a l practi cal c ompe t e n ce

Each student wtl l have to perforn1 a n u m ber of experiments durtnr.t each year. Ther e
are no n1ar1<s ror this acuvtty. All tha t has to o e l'ecorded Is the date and tllle or the
practica l. A s a s tudent, you will not know when you have d o ne one o f t hese t asks.
The r e are n o m arks for it - a nd ther e ts n o pass or fall either. All t h at the exa m board

• l"eQulres ts tha t you do a n"llnlmum of five or the Hsted experiments across the thl*ee
ureus or physica l, Inorgani c and orga nic chemis try a t 1\S and unot h er nve at F\2.
There Is n othlng y o u can do In preparatio n for these experi m e n ts t h at w 111 h elp you
..
to get a better g:rade fn the unit.

B Qua li tative observa ti o n

T h is Is n'la rked out of 14.
There are four expel."lments fo t· J\.S and f o ur f or A2. These ha ve Deen deslt;c n ed by
the Edexcel e x am i n ing tean'l . You w ill be Issued with a wor ksh eet ot the start of the
practtca l session a nd wil l have 1 h ou r t n whtc h to finish th e p r actical work . You wtll
be a llowed the edexce/ data bOoklet. If tt IS necessary, but n o no t es or other books,
I ncluding tht..s o ne. will be allowed Into the l aborntory. All w o rk n"lust be handed in at
the e nd o f the sessi o n .
T h e u nkn own s ubstances will be changed rrom year t o year. but t here IS l ntle scope
f o r c hango - ospocln.lly In organic chcn"\Jstry n t AS.
T h e focus of the tasKs ts you r skill at making: sen s i b le observations and n 1ost of the
tna rks wtll be a w arded ror this. YOu wt ll be expected t o ldenUfY the unknowns, and
the r e will be o n e o r two quesu o n s asking for e quations or types of r eact i on.
On ly o n e exper iment wt ll oo-.ant but you are a llowed to do two. three o r a l l four-on ly
t he best will score. vou al"e not a llowed to repeat any exp eriment.
This guide will h e lp you to pre pare f o r the assessment. You r t .each e r wil l warn y o u In
advance t h at you wil l be ctolnQ:. for tnstance. an AS t norQantc Qua l itative obsel"vattons

U nrt 3 and 6: Chemistry Labor"atory S kills

 assessment. You mu st prepare for the assessment by reading through the appropriate
pan of the AS or A2 Activity B section.

C Quantitative measurement:
This Is rnat·ked out of 14.

AS
There are two tttrattons and two enthalpy c hange expertments . As with Activity B.
you may do rnote than o n e - only the best wfll cour\l.
The practical work must be co tnp leted fn a I hour session, but you n'lay be allowed
t o do t h e calculation at a l ater time. 1rthls Is so. maKe su re that you know how to do
thts type or ca l c u tauon before the second session.

Tltrattons
over half of t h e marks a r e :lwarded for choosing two tl t res t h at are concordant and
for g-etti nQ the correct m ea n titre.
The utrauon will either be acid/base or todtne/thtosutn.ue. I n both you shoul d expect
to weigh out a solid. d i ssolve I t In water. transfer It to a volumetric flask nnd make the
solution 1.1p to 250cm 3 ,

Enthalpy change experiments

• The procedure IS stmllar In both experiment s. The reagents :are mixed tn a polystyrene
cup that Is held In o benker, a n d the. ten-.perature change Is n'leas ured. Thi s cou l d
..
involve either adding the second r e.ilgent In portio ns o r adding tt all at t h e same Ume.
If\ the rorrnee', a graph o r ternperature ag_atnst lime wtll have to be plotted.

The mujo rHy of t he m:.rks are for the accuracy o f measuring the temper~tures and for
dolnQ the O H,.••c u cm ca l culatton .

A2
The ro ur experiments at thl:S level are two utrauons and two klneuc expertments.

As wtth the AS Activity c exper i ments. the practtc.o l work n'lust be completed in a 1
hour session. but you may be allowed to do t he calcu tauon at a l ater ttme. If this Is
so. make s ure then you know h ow to do thts type or ca lc u lation before the second
session.

Tltratlons
The two experiment s ate:
( I ) AUtrallon Jnvo/vln[/ potassium manganate(vu)
As wllh tho AS lltrntlons . a soiJd has to be weighed out. dissolved, trans ferred nnd
made up to 250cm3. The potassfu rn manganate(vn) solution wi ll be i n t he butette
and no lndtcator Is needed becau se no n1.oce Is added when the sotutton turns pale
pink. over half of the marks will be for accuracy.

6 Ede><:Cel AS/ A2 ChEHY'Ii stry

 (2)A pll titration
Here a strong alk.a lt is added to a weak. a c id In s m all portions and the p H of the
solutio n t s n1easuted arter eaCh addttton .

Kinetic experiments
one o f these will Involve f o llowing a r eaction , such as the Iodination of propanone.
T h e oth e r Is t o m easu r e t h e r a t e o f r eactio n at diffe r e nt t e n1pe ratur es, a nd so be ab le
E x~ m i n e ...- c:-ip
to ca lc ulate the acttvatlon energy.
You w ill no~ be allovved
-to ta.kc -this c:u- ;;u,y book
D Pre paration (o"ther 1:han a data booklet)
Thts 1s marked o ut o r 12. Betng abl e to cal c u l a t e the percentage yield gains 3 n 1arks, or you r- notes i n~o the
with 1 0 1· 2 marks a vailable f o r obtaining a good yiel d In the exp e rime nt. labor:~:tc:11-y when you
are beina assessed. You
AS ar-e nO'l allowed t.o take
ovt :an y work f..-on-1 tha
T h ere ace three expertments - one Is a n o r ganic p tepacation and the oth er two
laborat:ory. even if the
I nvolve the preparauon o f anorgani C sa i ls .
asse:s:Sr'T'Ient is not rinished.
Your """''r"k will be aiven
A2 back to you when you
The r e are three e xpe rime n ts - two are o rganic p 1·epa rot1 o n s and the other I s the continue t:hc ::t.:ssessrnen-t ::tt
preparatio n of a so11d complex transition m eta l con1pou nd . a later -t-ime.

• ..

U nrt 3 and 6 : Chemistry Labor"atory S ki lls 7


• that you:
If you ;ou ·et :~o:ook.a;td to idQn ti(y
a substan ce. a Ne either
it.~ n'"'rne or i-t.s for n"' u ltt. If
you aive b oth t h e n bO'th
mus t b e correct. N a m es
a.-a e:~.sio •- 'th n n forrnu ln o ,
where mistakes: s u t:h a s
NaCO, or M QN O] are
c orTu"T"'o n . ~owcrvor; if you
are asked -f'or the (on-nula .
1.he n..t.me w ill not sco r"e.
8 Ede><:Cel AS/A2 ChEHY'Ii stry
Content Guidance
Content Guidance
Unit: 3
Activity B: Qualitative observation
There are four exper l n'lents th.a.t you could be asked to carry out.
<•> An observation exerctse on three tnorganic vnknowns.
(2) 1\n observation exercise on another three lnOI'Q:antc unknowns.
(3) An observation cxorc l.so on three organic compounds. probably lltnltod to nlkcnc-s
and a l cohol s .
(4) An obsetvauon exercise on two organic co1npounds, 01le probably being: a
halogeno:tlknnc.
If yo~,.a do more than o n e. each wtll be marked and you wil l score the one with t h e
highest tnal'kS. Each expertn'lent has a 1naxrrnurn or 14 tnarks.
Most of the ma•·ks a r e awarded for n,.aking the correct observatio n s, so make sure
•
•
•
m1x the ··eas;cents ptoperly before recordtnQ: colour chanQ:es
stale if there Is u precipi tate and record lls col our
n,ake sure, tfyou are asked to add a substance until tn excess, that you observe any
c hanges after· adding: a Jtttle as well as those after addln" excess
• state the col our before and aflet tf there t s a col o ur cha n g e - t f there ts no colour
chango. say so (rather t h a n say that there I s no renctlon)
• ln organic chemistry, If two layers forn1. say so
Inorganic substances
Most of the tnarks ate rot observations. You Wil l normally be expected to Identify each
solid and you may be t'eq utred to wrne an equauon, e.g. ror u thertna l decomposruot'\,
a redox reactlon or a p t·ect pitatlon reaction. A typlca I ma r k distribution i.s :
Obco rvatlonc 9 o r 10 IT'Ia rks
l dont;lf"i c;atlo n of" oac h unk n own 3 rnar kc.
Equation a n d/or comment I o r 2 m a. r k s
vou may assume that only the rou owlnQ: tons will be tested for.
C:at::IOr'l$ NH ....
Anion s
 Unlc 3

T escs on solids
Heating the solid
llydrogen c urbo natcs . .su c h a s sodturn hydro gcneilrbo nat e ( N uJoi CO~) , and s alts
co n ta ining w ater of c rys ta l li s atio n give o ff w a t e r v a p ou r , whic h will con den se in the
1.appe r p ar-t or t h e test t ube. For t h ese, t h e r e wnl b e a m a rk for o b se.-vt n g: t h e d r o p let s
o f w a t er nea r the mouth o r the test tube.
H eating the sol i d is a l so a test whi c h ind i cat es If the unkno wn I s a nitrate. a c arbo n a t e
or a tn m ontu rn c h toctd e .
Tho solid :sh o uld be hea t e d , gently at firs t and the n s tro ngly. L ook f o r s ublltno.tJo n
o r m e l t ing a n d wheth e r a gas Is e v o l v e d o r n ot. Y ou might b e tol d t o test the gas.
Possible observau o n s ma t'I<S a ..e s h own with a ~

Test Obser-vations Inferences

l-fe;.tlng a nlc:rat·• -
any gas evolved wah a
"'"' • M o lts V and chon glvo• off • It I s olt;.hor aodlurn nltr"":\te
bubbles of a eotourtess ps or potassium nlt.rate
atowtna epllnt which relights ftll" ::.. glowing
splint:
• M 4 1 ~c ftll" 3nd ~hen stv4s off.:.
b1•own gas ftll" and one wh i ch
• It le elch er ll~hlum n ltr3t.e
or a. group 2 t'lltrat.o
E x an'une r d p
Record whc'thcr.
reHaht• ftll" a. Qlowtna splln~ • it. melts or sublimes
Note: If tho solid I s a. hydrated • i t eives off w a ter vapou ~

•
nltrat.e. wacer/st:eam wtll also .a colourl o ss &:liS o r~
bo ob.corvod and w ill scor o n b 1"0Wn ~as •
mark
H eactna a ca.rbonate or
hydrogoneal~bonat;o -
• Orops of water condense on
upper part o f tho tubo ftll" n nd
• It I s a a:r-oup I
hyd rogo n ca rbonnto
test. any aas evol ved With a aas ts produeed whleh turns
l lrnowator llrnowotor milky ftll" (or cloudy
or gtves a whtce precipitate)
• (No W<ll~4r produc.ed but) "'
gas I s evolved whleh turns
• The solid Is 3 SI'"'OUP 2
carbonate or lithium
limewater milky ......- e arbonat:e
Ho;;;.clng .,.mrnonlufTI
eh l ortde
• Solid subllmos ftll" (o::u- solid
reforms In uppe,. pa,.t: of c,he
• It I a .;arnrnonlun-. chloride

test tube)

T h e eQuati o n for t h e t h erm a l decom J;>OSi tlon or pot assi u m n itr a t e IS ;

2 K N O..,( !S) - 2 K N 02( 5) .... 0,(8)

T h e eQuati o n for t h e t h e rma l deco m posi tio n or m aQn estu m n itr ate I S;
2Mg(N0,:,}2(S) - 2M&O(.s) .... 4 N02(8) .... ~(8)

Flame test
M a k e s-.are t h a t t h e wire Is c lea n by d tppl n s;r it i n to son1 e co n c e ntrated hYd r oc:h lortc
actd. a 1ld t hen p utting; I t rn to the h o t pa n or a Bu nsen n ame. R epeat u n ut the n ame I S
n o t col o ured .

U n rt 3 and 6 : Chemistry Labor"atory S ki lls 9

 Content Guidance

Exan·une.- c:ip Now dlp the "vlre Into con c entrate d hydrochlo t·lc a c id and then Into the solid~ and
You n-.u ::.t b o .::lblo to immed iate ly p lace it In t h e h ot p 3 r t of the B unsen fla m e .
d•st-.~ ntzu i lih bet.............e n tho
1:hr ee r ed names in this Colour I on r esponsl ble
t able :r;o as to be ll.blo to C r t rn 5on Lt*
tdent.tfy the ton, but t o Y o llow (not o r a.ngo ) N :l-
nd.me the a c::tua l colo u r you
Lilac K*
c::;an stata v.:arious s;h ados o f
Y e llow- r o d Cn2._
red - s u ch as ma ~ent.a for
lithiu m u.nd b riek-red ro,.. Red S r :l•
c:;alc::turn. Pale g ree n (or a p ple g ree n ) B a 2+

Addition or acid: test (or carbonates and hydrogencarbonates

S olid a roup 2 Whe n dilute hydroch l o r i c or s ulfuric a c id I s adde d to the solid. a gas n,ay b e e v o lv e d .
h ydroszon (:arbon;'ltA;,l$ d o
n ot exist. T h e td e nlfty or the c atio n m ay a l ready b e kno wn rr-om a na 1n e t est.

T'esw:: Obse rvations I nferences

A f:ld + 50IId a:roup
com p o und - '
t o st: a n y g a.c
• B ubblfu. V (or ffZ%1 n a or
ef-fervescence)
evol ved Wlt.h Hmewace r • L lmewacer t.urn s milky/
cloudy V
• It: I s a carbonate or
hydro g o n c:.rbo n :..to
F.xan,tnCIIr t i p Acid + sol i d g r oup 2
compound - t.esc any a:as
• Bubble s V (Or' nz.ztng or
effervesc ence)
ovol vod with llmowa tor • L i m ewat er t:ur·n s m i lky/
cloudy V
• It I s Q. c.a.rbon t'l.t.o

fi zz ina. -ryptcu.l cqunuo n s arc :

N a :z:CO,( S) + J-1 2 S04 ( aq) ._ N a 2 S04 (BQ ) + J-1 2 0 (1) +- CO.:z(Q)

To distingutsh between a carbonate a n d hydrogencarbonate

Y e sw:: Obse,.vadons I nferences
A dd s ome solid t o a .hnost.
b o lll ng wntor
•• B ~or bbles
(eff"e rvesf:on ce) . ,
Llmevvat e t· goe• m il ky V • It I S a h y d rogenear b onate
T est: any a u evolved wtth
llm OWI"t~r·

M ::ako " sol u cto n o f c h o • Elthor w hl to proclplti.'lt.t:o V • It I s a car bon a t e

u nknown and add cal c:lum
c hlo r ldo sohJt:l on
• Or' no preclpl ca t:e V • It: t s a hydr'OQ:enc:ar'·bonace

A dditi on o( sodium hydroxide: test (or ammonium salts

Whe n dllute s odi um h y di'OXt d e I s a dde d t o the soUd a nd the t est tube " ently w a rme d ,
a gas mny bo e volved whic h can bo tes t e d w i th damp red and dan,p b lu e lltn,us paper,
or with a glass r o d d i ppe d Into c oncent r a t,e d hydr och Jo rrc a c id.

to Ede><:Ce l AS/ A2 C hEHY'Ii stry

 Unit 3

Tesc Observat:tons l nt'erenc:es

Warn" wlt:h dlh.n:e sodium
hydroxldo nnd to.st any gas:
evolved:
• Qlthor with damp red 3nd blue
l l t .mus paper
• c;._,.s: "turns: red litmus: blue
..,... Blue l i tmus •tays blue ..,...
• Cas: Is: ammonia, co ft
Is an ammonium s alt
• or with a atass: rod
dipped l nc:o concontr:r..tod
• White smoke .,..... • White smoke le
arn~nJurn chloride. so It
hydrochloric a c id Is an ammonium salt:
Tho equatio n f o r t h e r e a c tio n o f ummo nln gu s with hydrochlorJc .ac id Is:
N H 3 (Q) + H C I (g) ~ N H 4 CI (5)

Concentrated sulfuric acid cesc for Inorganic halides E :xatvwi n eu- t:i p
T h is test is used to disti n guish betw ee n di f ref"e n t h a lides. T h e con c e n tf"ated acid I s l..ook fo r sto:;u 'T'I)" f"v rnes a n d
carefully add ed to the soltd. Thi s test m u st be don e Jn a r u me c upboard. a red-brown aas.
Tesc Obser"vac lons l nfer·enc:es
Add the acJd to a chloride
3nd ~et any g;uo evol ved:
• Bubbl es .....-; scearny (or • Hydroaen chloride
evolved
rT'IIsty) fumos: V ovol vod
• either wlt:h a g l ass rod
dipped l1"t concentrat:ed
(do not s ay white smoke • It Is a chloride
here)

•
ammoni a
• Whlt:e Sn'\Oke V
or with damp red and with
• Red lltn-u.•• scayc red .,.

• d :unp blue Utn'\u.c papor

Add tho ncl d to a. bromtdo •
Blue lltmu.s goes •·ed .....
Steamy fume• .,..... and red-
brown ps: .,.....
• .-.ydrogon brornldo
evolved
..
• Bron'\lne evol ved
• It Is a bromide
Add the ac.t d to an IOdide Any two of:
• S teamy f\lrnes: • H ydroaen IOdide • H I
• Purple vapour • Iodine
• Yellow solid •• Sulfur
• Bad ogg srnolllng s:ns ~ydrogon s:ulftde, H 2 s
• It IS an IOdide

T est:s o n so lut:io n s
Addition of acid/ned sliver nitrate solution: the halide test
1\ f e w dro p s o fd t luto nltl· t c acid u ro c:addc d t o tho unknow n solullo n, f o llo wed by n f e w
d r o p s of s live r nitra t e solutio n . The sol ub ility of t h e preci pitate f o nned i s the n tested Look fo r :1 w h i-to o r ci""'Clnrn
t n dilute and con centrated a m mon ia . o r yel k:lw preciprtate.

Tesc O b servac:lons I nferences

Add dilute nttrtc aeld co a
solution of tho unknown and
• Whtc.e pr'4iJ!clpltaUt .,. "turnln.a
purple on stilndlng.....; soluble In
• It IS a Chlor-Ide

Che•"t sliver nitrate dilute ammonia .,.

Tact the P~"'ec: l pltatet fir s t
w i th dilute ammoni a and
• Cronm procl pltate ..... lns:ol ublo
tn dilute but soluble tn
• It I s n broml do

then (If no chanae) wlt.h concentr9~ed 9mrnonta .,.

concontl~iltcd et.rT'Irnonl a
• Yellow precipitate .,. Insoluble
In c:onc:en1:-ra.t:ed ammonia. .,.
• It • • an IOdide

U nrt 3 and 6 : Chemistry Labor-atory S ki lls II

 Content Gui dance

The t o ntc e quatio n f o r the precipit a tio n o f a s i l v e r h a lide ( X s t a nds fo r C L, Br o r I ) l s :

Sornat.imes the &ilvctr
A g-(aQ) + X-( <3Q) ~ A gX(S)
n i tr•ate is added firosl..
followod by the n itnc a cid.
The observation s (o ,- a Addition of chlorine water
c:hlo1ide t.hen are d. w h i te
Thls t s u r e dox J·cu c tlo n tn whic h tho c hl o rin e o x l dts c s the unkno wn.
procipitnto --' ~ich stays
on add1t:ion of n itlic a cid .....-:
T esc Observation s I nfe r e nces
A dd a r ew drops or c:hl orl ne • B rown (or y ell ow) • B rom i n e o•·
IOdi n e
wa1:.er •olutlon V produced
T hen a d d sc:..rch Golutlon • Goes bl u o - bt~ck --' • It Is an Iodide
• Ooes not ao bh.1e- bla.c k V • It liS a bromide

The ton ic half- cqua.uo n f o r the r e duc uon or c h l o t· inc I s:

C l 2(aq ) -+ 2e- ~ 2CI-(aQ )

Addition of acidified barium chloride: the sulfate test

J'\ f ew dro p :s o r dilute h y drochlo ric a c id a r c uddcd t o the unkno wn solutio n f o llo w e d
by a few d r o p s o fb a rh.1m ch l o r t d e solutio n .

Obcorvat'lon c lnf"o r a ncc c

Whl t.e preet pl u..~e V I~ Is- n c ulfat:o

• The ton tc e q uauon f o r t h e preci p i tatio n o f b arium su l fate Is:

a a~ • (aq) + s o4 :2- (aCI) ~ e a:Se>4 (S)
..
Sometin"'les the badum
chlon dc is ~ddod Test for nitrates
first:. (ollo \NE!d b y t:h e In t h i s t est t h e nitrate Io n s a r e r-e duced t o a n"l m o nta gas .
hydr-oc:hlof'ic: a cid. T he
ob~rv;,1rti Qn $ t hen :c.r Q T Q ct' 0b G$ f"V~t'ion c I nf"o r o n coc
w h it.e p r eciprtat:e V Add Dov:..rdn' c a lloy (or n l umlnh.n n •
whic:h ~l.:\y!!> on add i t ion o f
h)'Circx:hiQI;C: ac;id .......:-
powder) and d ilute sod1u 1n
hydr oxi de ;)n d w-3rrn - ""'8t ;;tn y g:a.s
Bubbles (efforve~Jcence)
""
evolved:
• e i ther With a g l ass: rod dipped tn
concentrated hyd roch l ori c ~c ld
• W hl1:.e smoke V • It IG ~ n lt: r <"~Q

• or w i th damp red litmus • Litmus aoe• blue V

Test the solubility of hydroxides

.J'\11 stou p 1 h y dro xides a nd barium hyd r oxtde are soluble tn wat er. M agn es 1u1n
hydro x i d e Is In sol u b le and c alc i u m hyd r o xide s lig h tly solubl e.

T oct' Obco rva-tionc I nf"c r o ncos

Add dll uto •o dh.•m h yd r oxldo • Whlt.o p roclpltill t o --' • I t Is a m agn os1u1n
t.o a solu tiOn o r the u nknown
• S light whlce preclpl cace V c:ompou n d
• It Is a calci um co m poun d

12 Ede><CQI A S/A 2 C h Qmlstry

 Unit 3

The Ionic equ a u on for the preclpltatlon of rnag n esi un'l hydroxide. for example. I s:
Mg2•(aQ)-+ 20H-(aQ) ~ MQ:(OH):a(S)

Addition of zinc or magnesium

I f the unknown is an acld, such us dilute su lfuric ac id, hydrogen wiiJ be produced.

T est O b ser vat ion s I n f e r en ces

Add 'Zinc or n1a.gnoslurn t o a
solut.lon o f t.:he unknown and
• Bubbl o15 (of-fervescence) . ,

wnrrn
Teet. any aas evolved wlt.h a • I gni tes Wlt.h a s queaky
pop . ,
• lc 1s an acid
burning splint.

The Ionic eq uauon for the reactton or magnesium wllh the ucJd t s:

Mg(s) + 2H•·(aq) - Mg2._(aq) + H:z.(Q)

Kn o wledge> c h~ c k I
Assume;, t h at you h avta l;x;tc;,n a'vc;,n s.on-~o solid poU1ss:iurn hydi"'Qac;anC".O'•-bon a1;o.
W riut down t h ta obs.ci~tions: t h at yov would QX"ptac:t to n-~ak.e if you c:ar •;od out t h e
followina test-s.
(a) Carry out a name test o n some of t he sol id. Write down you r observations. (I)
(b) Put some o-f t h e solid in a. test t ube a nd heat it in a Bunsen f lame. T est the Qas

• (c)
evolved w it h l in-~ewAter. Wr-i-te d own you,-. observatio n s.
Make a solution w i th -the rerna.inder o f ·tt.,e solid and addS di"'Ops o f e.alc iurn
c hlondo solution. W r itct dc;tl..v n your observations.
(2)

(I)
..
(d) Usina )"'0'-'r obsorv.:.:t:ion s:, wnto t h o fo....,...ula o f 'tho unknown solid. (I)

Organic substances
T h e o nly types of com pounds exa n'lln ed I n the AS chemi stry course are:
• hych·ocarbons- such as hexane and cyclohexene
• alcohols - lncludt ns primary, secondary and tertiary alcohols
• h aloge n oal k a n e s - rn clud lng c h to r o-. b r o n'lo- and todoalkanes
N ote that tr you cto an orQ:antc assessment bt:;fore you have s tudied ha logenoa tkanes,
then t he unknowns arc ll n'lltcd to hydroca rbo n s nnd alcohol s.
A l ways: road -tho q~curti on
A typica l mark distribution is: care ful ly. It m iaht stat e
-the nun-~be •- of ca.rbon
O b serva1:1on s 9 or 10 mart«: ;nom s in n-~ o l ocul os: o f
tncer- pre1::1na mass or I R s:pec1:r a I or 2 marks the unknown s . o r t h a t
tnc erprecl ng obse-r-vat:lons I o r 2 marks -t"'"-'C o f 'tho c ornpo '-'nds

l dent:lfylng unknowns 2 or 3 maf'ks

are isomers. o r that o n e
con't.ains a branched
Possible observa u o n s marks are s hown w i th a ...... c a-r b o n c h a in.

U nrt 3 and 6: Chemistry Labor"atory Skills 13

 Content Gui dance

Comb u sti on
The unknown Is piD.ccd on a cruc ibl e lid <:and Ignited wlth n lighted s plint.
When n-uxinQ an onza.n•c Observation s I nferences
li ~uid with an aqueous
It burns with a clear non ..smoky fhune ~ L ow C;lrbon-to-hydrogon ratio could bo
soluti on, look to sao an alcohol
whet:he•- one or two l ay ers
lt. burns wlt.ha smoky f lame V High ea.-bon-co-hydrogen rati O - - probably
~u-e formed.
1<11 c;ycllc ~lkano o r cyclic ~ l kone

Addition of water, followed by universa l i ndi cator so l ution

or p H paper
l:xan111nC!'r tip
At AS, lhis tesl shows 1-hut The unk n o wn ts added t o som e water in a test tube a nd s h aken .
t h o unknO'W I~ i10 ;;tn .-l cohol.
T esc Observations l nf"cu·en ces
CarboxyliC acids also .Qive a
posit-i ve .....ezuh.• but -Lhey r.u-c Add t.O wat.er • Elttuw ~wo layers form ~ • I~ does: not. hych~oaen-bond
with w:.tor
c:o'VQretd in A2 not AS.
• Or tt dissolves fully V • It hydroaen- bonds wlc:.h
Add a. lltt.lo uniVOI'"CQ.I water (a.nd tc a.n alcohol)
lndlcat:or • Green col our V • It IS a neutral substance

A primary alcohol has one T ests f or a C = C group In alkenes

carbon ;::a1:orn ::.tt:-.chocl Obs:er"vatJon s l nfer"ences:
Yesc:

•
-co the -COH Qroup, e .Q.
propan- I -of:
Add some bromine wac;,e•• co t.he
unknown- sc:.oppor tho cost c:.ubo
and shake caf"efully
Brown bromine wat:er aoes
c-ol ourless V and two layers
are formed V
C - C aroup present
..
i I 'i'
H--c--c--c--OH ..
Add dilute s ulfuric acid then Purple solution goes C•C group pre•ent
pocas:slum manaanace(vu) solut:lon colourless V and cwo layers
,!, ,!, ,!, - - •h;:.ko tho eost tubo or warm
In a beaker of hoc wacer
a.ro formod V

A s.ec:ondary a lcohol
has 1:Wo ca1--bo1"1 atoms T ests for an OH group
~tt4chod -to -tho COl I Yest Observations Infere nces
Qn:>UP. e iZ· ~u-opa.n-2-o l :
Add a small piece of sodium ~ t.he • Bubblos ovolvod ~ • It concalnS: an O H
•
H-~-b-f-H
unknown In an cv:.por:.tlng basin Sodium diS-appears or• a group
whlt.o colld foriT'Is V
•
bH H H
Add colld phosphorus(v) chlor·l do
and test any gas evolved:
• elt.hor wlt.h a slass: rod dipped In
•
•
Steamy furnos ovolvod .,.,

Whlt.e smoke formed V

It conc:..,.ln • nn O H
group

A terti ..u-y ulc:ohof hu~ concentrated ammonia

t h roo c:;:r,rbon ~:torn$ • or wl·t:h damp blue llt:.mus: pg_p er • L.ltmue aoes red V
attached to -the -COH
gn:>up. c.ijz. ITiethylp•-opan- Oxidation to differentiate between tertiary and other alcohols
2-of:
T es:c Observations Infe r e n ces
CH, Add dilute sul furic aci d
and aqueous potassium
• Etthor tho oro:tngo
solution turns green ~
• l t. Is a prlmo:try o•· a
secondary a l cohol
H ,C--"=--CH
I , dlcht·omat.e(v•)- t.hen warm <he
mixture In a beaker of hot wate•·
• Or t.he solut.lon cca.ys
orange V
• It Is a t.ert.lary alcohol
OH

14 Ede><CQI AS/A2 C hQm lstry

 Unlc 3

T escs for h a logenoalkanes

You may be u .skcd t o test the so lubility In water - hnlogcnonlkancs nrc Insoluble,
a nd so f o rm t •wo layer$.
vou may be asked to hydrolyse the halogenoalkane t o an alc ohol, and then test for
the halide i o n produced.
You m ay be asked to ca rr-y o ut a n elfmi n atton reac tion (on ly wfth sec ondary o r
tertiary halogenoa l kanes).

Tesc Observations I nferences

Shake a f&.H df"ops of the unknown
wlc.h waGer
•,...,.,o layers form .....
Add a few drops of et.hanol and
•• Whtt.o prectpiUt.o V" • It: contains a c Cl aroup
:..quoous sliver nltl"'i1to nnd dlluto Cream preci pitate V" • I t contn.lns Q. C - Br group
ntt:rlc aCid - - st.and the test. tube In
a bonkor of hot water
• Yellow preclpl"te .,..... • It: conc:alns a c -1 aroup

Add <4 dropc of ethanol and t.hon • Whtt:o pr"oclplt.:t.to V • I t cona.tn•;. c

2 em;) of dilute sodium hydroxide
- - S;~nd t.he t.esc tube In -a beaker
of hot water for S minutes; then
Clgr ·oup
• Cream precipitate .,..... • It: contains a C-Brgroup
• Yellow proc lpi'U)(;O .,..... • It concalns a C -1 aroup

add excess nitric acid followed by

The equations for the
n.quoous. sl lvor nitrate
action of nqucous silver
Add concontra.tod sodl u,.. • Brown bro,..lno goo• • J-1- h:.logon olln-~lnated
nit:ra~e are:

•
hydroXIde In ethanol - f1t t:.he test:
tubo wt'th 9 delivery t:ubo 9nd w;arrn
gently. pas.s1ng any gas evol ved
through a little bromine W3ter
colourl ess .,..... for1n1ng an alkene
R-X + H 20 _. RO H
H ... -... X tl'\en
x- + Aa• -.. AaX
..
The ldontJl y of lhc halogen In lhc precipitate forn,cd wllh s li ver nltrnte cn n be
confirmed by adding ammonia solullon .

Obsorvatione l n-f"oroncoe
Precipitate dissol ves. In dlfUtO I UTII"nOnlo::t ....... AgCI <he unknown lc A c:hloroalkano
Procfpltate fneolublo In dilute but colubfo In AgBr tho unknown l c ::\ bro,..o:.lkano
cone.enuoated ammonia .,.....
Precipitate Insoluble In concentrated AgO the unknown ts an todoalka1'\e
ammonia .,.....

M ass speccra
Look rot the rou owtng.

Peaks I nferences
At m/e - 29 or at (molecular lon C 2 Hs gi"''up tn the mol ecule (at A2. this peak
value- 29)* could also be caused by C J-10 In the molecule)
A strona peak ac (M I}* Caused by loss of H from an alcohol
Molecular ton doublet of equal lnt;ent:ltles M olecule contain• one bromine atom
:.t two 1T1/o units apart
Mofacul.ar lon doublat fn ••:atlo 3: I at two Molocuto cont.-..tns ono chtorlno :ato,..
mle untts apart

U n rt 3 and 6: Chemistry Labor"atory S ki lls IS

 Content Guidance

•Fo•· cx:l.l"nplo w ith prop:an• l • o l (Mr - 60), ;:a pc::tk a-t rn/c - (60 - 29) - 3 t c..ausod by the
CH-,OH,.. ion and a pe;~k at:. (60 - I ) = 59 caused by t:.h e C 2 H 5 CH 2 0 ... ion.

You muy be asked t o work out the number of carbon atoms. and hence the rnolccular
forn'lula, from the value of rn/e for t h e n'lolecular ion. For exampl e, an alcohol that IS
noc oxtdlsed by acidified potassh.•m d lchromate(vl) has a m o lecu lar i on peak or nl/e =
74. lhe O H contributes t 7, t eavt•'S ~7. ThiS ts made up or 4 carbon atoms (4 x 12 = 48)
and 9 h ydrogen u.toms, so the unknown Is:
IH,
t-t,c--y--ct-t,
OH

Infrared spectra
vou wtll be allowed to use the .edexce/ data boo.k.Jec to look u p the rcequenctes a t
which bonds nbsorb, so you do n ot neod to learn these values. At AS, this will bo
limtted to the v~lues lfsted In the fol lowtnQ tabl e .

B o n d A bso .-pc.l on -fr eque n cy/ern -•

c H In a .lkanes 3000 2853
C - C In alkenes 1669- 1645
0 -H In alcohole A broad peak at. 3'750- 32.00

• The o - 11 peak Is broad because of hydrogen bonding.

Kuowl cdgc:o c.h eclc. 2

A.s-sume the~.t. you h ave bee1., aiven sor-ne liqui d 2· ~-thylpi""'pAn -2-ol. VV'1·i te down <the
obsorvation s. th~t yov \I\.I'I!Qul d axpec:t W make.
Cor-npovnc:f X has rnoloculets <that con tain 4 c;;:.rbon :atQrns, Coarr-y out tho followin8 tetsts on
compound X.
(a) Pu~ 2cm3 of water in a test t.ube and add an equal 'IIOiurne of X. then add 3 drops of
universal indicator solu~on. VVr"ite down your observ::.t:ions. (2)
(b) WorkinQ in a fume c upboard, p u t I cm3 of X in a test t:ube and add t-.aff a spatula full of
phosphor-us.(v) c:h&orid et and tet&t any aas evolved with da~T~p bluet litm us. paper: Writet
down your observati ons. (2)
(c) To I cn"'' 3 of X in a test tube add an equal 'IIOiurne of dilu~e sutfuric acid. followed by
6 d.-c p s of pcrtassiurn d ic:hr"Or-nnt:e(v.) solution. Stand t he tes-t tube in n be:1ker of kat
water for S minutes. Write down yo1,1r observations.. (I)
(d) l..ook at t h o spectrum bctlow anc::l identiiY <thet bonds retsponsiblo for- the peaks
labelled P and Q. (2)
(e) your"" obse.-vations, and me infor'TY\ation Qiven. wr""i"te the ske/er:ol formul a of
Usin~
compound X. (I)

16 Ede><:Cel AS/A2 ChEHY'Ii stry

 Unit 3

100

i
J 50

~oJ~o~o-.~~.-~-.-.,~
o~~~-.-.~.-~2~000
,--,~-.--.---~~-soo
.--,--~--.--,--~-o.--.--~--.­
oo
w a.venurnber/crn-t

You rnust n~con::l: You must look f or:

• the cotour before and after t:he tQst droplets ofwa:ter condenstna on t he upper part of
• the coto-ur of any predpltate the test tube when heating a solid
• whether: In organic tests. t:wo layers foi'TY"l • b u bbles o f gas evotved w h en adding an acid
A lways sh ake t:ne test tube "thoroughly'Wt'len mixing

• Activity C: Quantitative measurement

two solutions.

Full details of all the experiments assesstng this activitY will be given to you Just
before sulr u ng the assessment. n rs es.senual t ha t you read the det ails carefully
before starting any practica l work.
T here are four experln'lerns t hat you cou l d be asked to cai"ry o ut:
( I ) an ucld / ba.sc titration
(2) an lodlne/sod lun, thiosul fa te titration
(3) an expert n'lent to find the enthalpy c.hanQe or a sfnQle reaction
(4) an expertment t o nnd tl\e ent halpy chanQe ror two reacuons, and u se the results
und Hess's l aw t o ca1culato the enth a lpy change for a third reaction
rfyou do •no•·e than o ne experfn1ent, each wtl l be marked a n d you will score the one
wnh t he highest marks. Each experfl'neru has a n1ax1mum or 14 matk.s.

Titrations
ove1· h alf of the marks are awarded for choosi n g two tit r es that are con cor dant (n o
n1ore than 0 . 2cm~between the la r g:est and the smal l est) a n d for g:ettl n s;c the correct
n1ean l llte. Thl.s rneans that the most lmpottant sk ill s are:

U nrt 3 and 6: Chemistry Labor"atory Skills 17


You m u :Sl reeo1-d tl'le
m asses and the ~iah t
of t h e solid to 2 decirnal
pl.a.ee1 T hus ., n"l:::t.ZS o f
12.30a must be recorded
as 12 .302 and not 12.3a..
Knowledg~ ch~c:::k
Use "the data bel ovv to
ealc::ulate the 96 ei'T'Or" in
weti_szhi'"'8 ;l solid.
of bottl e on-1pty =
2
of bottle +- sohd =
2 ..... 1 6~~:
18
Content Guidance
• welg:htng out t h e solid and m;;.ktng up 250cm~ of solutton
• dotnQ: the Utl"aUon and knowing the colou r or the Indicator at the end potnt - If
you o:a.rc add i ng a l kali fron'l the burette, s t op when phenolphtha lein goes just pink
or when m ethyl orange goes ora nge .
There ure two types of tltrnuon:s that cou ld be :set :
• acid/base
• Iodi n e/thiosulfate
For both types the n1.ark d l strfbuuon Is approximat ely:
R e cording of" masses and vol un"tcs 2 or 3 marks
Accuracy 7 marks
Calc ula~:io n 3 o r .,. m:~o rks;
Cornrnet n c: I o r 2 mOllrks-
YVe lghlng
You will be supplied with u weighing bottle containing a solid. You must weigh this,
using a balance accurat,e to 0.0 1 g. The solid Is then tipped i nto a beaker and the
weiQ:hlnQ: bottle cewelg:hed .
:J
Tho solid wil l thon n eed to be d issolved in water and tho so lution poured, using a
funnel, into a vol umetric flask. The beaker and any glass rod used in dissolving t h e
solid must be was11ed. with the water g:otng: tnto the volumetric nasi<.. Thts Is then
n,ade up t o Lhe nuuk with di:Slllled water und thorou ghly shaken. I f the shak.lng IS not
done properly, inconsistent tltres will be obtained and mork.s wil l be lost.
You now have two solutions - one made by dissolving the soUd. and the other
supplied by your teacher.
Erro r s t o a v o id in a t i tratio n
• General. Make sure thnt you read the ins truction s car e fully before starti ng the titration .
For a cid / base tttratlons. son1e Indicator fs added to the conical nask. In Iodine/
thtosuU'ate ttlratton.s. actd 1s added InHralty and the starch Indicator must not be added
until the iodine colour has faded t o a pale yello'\V (straw) colour.
• Pipette. This must be washed out with a little of one solutt on and
then 2~.ocm.;, ptpet ted tnto a contcal flask. Make sure tl"'at thel'e 22
nrc no air bubbles In t he s t em of the pipette whon you a1·c doing
this and that you use the correct solution .
• Burette. ThiS •nus t be washed oul wfth lhe other solution. I t Is then
filled to jus t above the zero mark, and liquid l:s run out until there 1:s 23
no air In the stonl. The funnel n1.ust then be removed from t h o t op
of the burette berore titrating. The inttfal volume fs then r ecorded .
• Recording. You must read the volume by ustng the l evel or the
bottom of t h o meniscus as shown.
Make sure U'lat you rec01'd the nnal and l nltJa l readings In the correct rows 1n the
table. The tnltlal reacUnQ 1nay be o.oocm 3 , but never .oo.oocn1 3 •
The tltre Is the diffe r ence between the Onal and the initial volumes.
• All volttme readltlSlS and lhe Utre muse be recorded co o .oscn1.;,. Thus the readfng In
the dta.gram above t.s 2~. 70 C m 3 , not 2;:!,.7 cm 3 and ceruunly not 24.~Cm 3 •
Ede><:C e l AS/A2 ChEHY'Ii stry
 Unit 3

• consistency. You mus t do repeat tttratfons unt il you get at least two that are concorda n t.
This m ean s that the difference between them m1.1St be 0 .20cm 3 or l ess. In the table
below. tltrauon nu•nbers 2 and 3 are the concordant tlll'es. and these are the ones that
m u st be averaged to give the average tJtrc thnt you will u se In the calcu lation.

Tlt:rat:lon numbe r
Buro t:-t::o roadlns (flnal)/cm 3
I
2 ... 15
2
2 S . OS 27. 10
3 ..
2 S . SS
(;xami n car t-i p
Rememb e r 'tO record a ll
Buro t:-t::o roadlns lnlt:l a l /c m 3 0 1.2 0 3 . 1S '2.00
you r 'VOlu mes to 0 .05 em' .
ff yov h a.d w ritwn t h e
Tlt:ro/crn3 '2.-4. IS 2 3.9 5 '2 ~.95 2.3 . 5S mean tit re as 23.9 cm3 o r
u se tlttatlons 2 and .3 to ca l culate the mean: the fina l readin & in -titr-atio n
3 as 27. 1 c m l. you '-""'uld
menn (average) titre 23.8~-+- 23.9~ - 23.90cnt3 have lost a mar k.
2
M arki n g
• Weighing. There fs 1 n1ark for r ecof'dlnQ a ll the masses to 0 .01 g .
• Accu~ttcy. There are 4 marks for Qet ttnQ an accurate mean u tre. If your value Js Exauune r t.i p
z0.30cnt 3 of your teacher's value, you will scor e 4 marks. I f you •· value I s between If t h e re is n o weia h in a
.:~o: O . ~O a nd ,.,_Q ,40cm 3 away fron1 your teacher's vaa~..e. Y0\.1 wfll sco r e 3 rna d (.S, rfyou in 'I.IOived, you w ill need to
are mote than 0.7ocm 3 from that val ue. you will score o for accuracy. aet within ± 0 .2 0eml oft.he
• Range oftJtrcs. There arc up to.,:, marks for h o w concordant t he tltrc.s arc t h a t you u.scd totlc h ar' s tft.rc, t o score 4
to ca lcu l ate the 1n ea n . I f they were 0 .20cm3 apart or less, you will scot'e the 3 n 1arks. t f m ark s.
the tttres In expetln1ents 2 ana~ In the table above were used to calculate the n1ean.

•
the runge n1ark wou ld be 3. I f tltrotlon 4 had a l so b een u sed, the dlffet·ence between
tho larges t (23.95) and t he smallest (23.55) I s 0.40 en'\~ and only 1 rnnsc mark would
have been scored . If titration 1 h ad also been Incl uded. the difference or 0 .90cm 3
..
would have resu l t ed In .,o l"ange matks betng awarded. This lllusttat es that care must
bo taken t o c hoose two o r more tttrcs with orange of no rno rc than 0.20cn'l~.
K nowl edR e c:h ec: k 4
Commen't on 'the errors in the following:

M ass o r wei g hin g bo c ~ l e + solid 12 . 3 g

M a.ss o r wei g hin g boc~le e.-n pt:y 11.2 g
M ass o r solid l. l g

Commen't on 'th e errors in 'the followina::

T lt:r at:l o n
Burc t:to r c adlns fln al/c,-, 3
I
2 3 .1 5
2
2 3 .5 0 1 5 .85
3 ..
22.2.5
l<.u owl e d ge c.h ec.k 6
Cale ula.te t:he pen:entaSte
Buro t:to r o adlns ( l n l tla l ) /c m 3 50 1. 20 23. 50 0 CITC)r in "t:rtr.:t-tion 3 ::lnd,
T lt:r o/cm 3 2 6 .S S 22. 3 2.2. 35 22.2 5 by compar·insr it wi"t.h the
96 e,-~,. in weiQhina in
Mean uue
. = (2""2=..::3c_:+_,2~2~.~33=5=+==2=2~2=5~)....::.::::.·:~~:~~--- Kno"""ed&et c:hac-k 3 o n
paae I 8. cornmen't on 'the
main ~ouree o r eri""'r.
A c id/b ase t:i t:rat:i o n s
T h ere nrc two like ly types of calculatton that you may be required to cun·y out, but
both sta 1·t Jn t h e sn.n'le way because both h ave a s Jmiln r experln'lentul m eth o d .

U nrt 3 and 6: Chemistry Labor"atory Skills 19

 Content Guidance

Remembe r:
rn ~s.s
•
1
""' 0 $ $= m olar m ass
• n-.o los = concc;antr->'t ion
in rno ldm-3 >t volu me
in ern3f1 0 00
Cak:ulate the n u n"\ber
of rnolos of solu-to
1n 2.3.45 c m 3 of a
0. 123 l"'nnI dm-J sofu'lion.
26.54 cm3 of a solution
contAined 0.00147 rnol.
Calcu la'te its concen'tration .
Calculation to (lnd the molar rnass of the solid
The n 'leth od Is to weigh out the solid, A, a nd use th i s to m ake up 250cm~ of solutio n .
This Is then Utrsted ag:al nst a standard soluti on o f B .
The c a lcu lau on t s best broken down Into step s.
( t ) <=n l cu lato the a rnou nt (n'loles) o f substance in t h e mean titre:
number o r 1noles or a = c onc entration of' R x: mea n titre
1000
(2) u s c tho stolchlo tnctry t o calcu l u t o tho omount (n'lolc.s) o f tho solfd dissolved In u
2S. Ocm ;:, sa mple. a n d h ence t h e amount I n 250cm;:,:
number o r motes or A = l \un'\ber or 1\ Ln equatton x moles of a
1\ u mber or a tn equation
Henc e . the nu1nber or m o tes or the solid tn 2~o cm 3 = 10 x above value.
(3) u sc your answer to (2) and tho m uss o f solid u sed to calcu l ate the molar n 'lass of
the solid:
n 'la:ss of A u sed
molar 1nas s o r A = answer to <2 >
Kn o w l e d ge <.h ec:.lc. 9
I.S3a of a diba.sic: aeid, H2X. was weiahed o ut. dissolved i n water and t.he .solu t ion 1"'1"'\ade up to
250cm'l w ith d is-tillo d w:.'tctr.
2S.Ocn-.l p o rtions o f this solu-tion woro -tiu-~tod ;:la:t i n~t 0. 111 n-.ol dm-J sodiu n-. hydi"'OXtdct

•
solution usinsz phenolphthalein indicator. T h e mean tit:re was 2 1.90cm3 .
T h e equation for the reac:-t:ion is:
H :z.X(aq) +- 2Na0H(aq) _. N a,2 X(aq) +- 2 H 2 0 ( 1)
\.IVha't •s the molar ma.ss of the~a~c;::;
;d::..;H
-"'~X7
...;;_____________ (3)

Calculation of the number of molecules of water of crystallisation

Th t s Is Lhe same a s the melhod In Knowledge chec k 9. except that an extra step has
to be ca rried out.

Knowl edge c::h ec::k 10

4 . 1 I a of hydr a'ted sodium carbonate. Nal.CO;t.XH:tO. was weiszhed out. and d tssolved in water.
T h e solut ion was made up to 250cm3 and 2S.Ocrn3 portion s vver e 1:it:r a'ted aaainst. standard
0.123 moldm -;1 hydroehloric: a.c:id ~na methyl or-anae as the indieator. The mean ·tiu-e was
2 3.4S c""'J·
T h o oqu~ti on for -tho ro;;ac:tion is :
Na2CC>:J(.aq) +- 21-lCI(:t.q) -... 2N:aCI(.aq) + C02(&) + '2H20(I)
C.:llcul:.to:
(:..) t h o arT'Ioun-t o f hydroch loric: a.c:id in tho rno:..n t iti'""CC ( I)
(b) tho ~ount o f sod ium c:ar bon :!'tc in 2S.Ocml, :..nd hence tho :1rnount in 250c:rnl (2)
(c) -tho rnol~ •- IT'Hio~ of t h o hyd~to d sodium c::u-bon .:ato using your ;1nswcu- t o (b)
a nd the mass o f hydrated sodium carbonate ( I)
(d) "t.he n u rT'Iber- of molecu les of wa'ter o f crystallisation in Na2CO, .xH 20 usinsz
you r answer t.o (c) ( I)

20 Ede><:Ce l AS/A2 ChEHY'Ii stry

 Unit 3

l od i ne/t:hlosul fat:e t:lt:rat:lons

The method Involves a solid ox idising agent being weighed out. d i ssolved In wo:atcr
a nd made up to 250c m ~ . Alternatively a n aqueous solutio n o f a n oxid is ing agent,
s u c h as hydr"OQ:en petoxtde. H aO.a. may be supp lied .
25cm,:, portions of the oxidising agent so lution are plpotted Into a conical flask and
an approximate v o lun'le of dilute su lfuric ac;ld added. £xce_c;s potassiun'l Iodide Is the n E x •min., r t:tp
added- thls reacts wlth the actcHrtec& oxtdtslnQ: ag;ent to liberate IOdine. If starch is added too
eal"'ty t he oomple>e will be
Tho Iodine produced ts then titrated against a standard soJuUon of sodium thiosulfate until
fcu-~d ir n::rvor-sibty .and t h o
the colour fades to .B pale yellow coi01.tr. Starch Indicator Is then added a n d the sodium titre will be inaccurate.
thto.sulfate added dt'OP by drop uruu ll\e blue-black starch/tocune compl ex goes cotout' less.

The equation for the oxidation of Iodide Ions and that for the reaction between the KnowledRe c:hec:k II
It berated Iodine ~nd thiosulfate Ions wtll be g:fven .
The concentration of a
The reacuon between the oxidisi ng agent. OA, .and excess IOdide I ons I S: solution or dichrorna'te(VI)
ion s;, cl"'2o?- c;o:~n bo found
yoA(aq) -+- 2zl-(aq) - z ·l 2 (aq ) • by addina excess po'tassium

so the amo unt of the oxlctl.slng aget\l = tnoles of 12 x:

T h e r eaction bet\.veen t h e libe r ated iodine and thiosulfate io n s I s:
iodide and t i'tra:tina the
libo,-..,"tod iodino with
sodiu m thiosulfate.
Cf'l072- -t- 14H..., +
61- _,. 2c •.3~ + J l2 +

• so the a m ou n t of 12 - V.. w the n'lo les

The calculauon t s best broken down tnto s t eps:
52 0~2- ,
? H20
C a lculate 'the r-a:~io
of "thiosul fate ions to
..
( I ) ~ leu Jato tho amount of sod I Lam thlos uJfato I n tho mcun titre: cht"'OITiato(v'l) ions.
motes or thtosult'ate =concent ration x m ea n titre
1000
(2) cal culate the amount of todrne liberated. and hence the number or moles o f
oxidising agent In 25.0cm,:
motes or tocttne llbet·ateel = Yz x moles or thlosulrate
moles of oxidising agent I n 2S.Ocm, - moles o f Iodine ~ :

0.85 iZ o( a szroup I rTletal iodate(V). MIO,, was """'9i,ah ed ou"t. dissofved in water and made up
to 250 eml.
25.0crTI' portions wer-e p ipet. ted into a conical nask and excess potassium iodide and d ilut:e
sulfu ,.;c :acid :addoc:l.
Tho libon:rtod iodin e w:.s 'titrnu.d .apins't 0 . 1 I I n-~ol d., -l sodium thiosulfato solution.
Tho ~n t it i"CC wAs 21.50c.,...l.
Tho equations fo r- tho reactions :trc:
1 0,-(~q) + S l -(~q) + t.J-l•(oq) -> 3 1,(oq) + 31-1,0(1)
J,_(a.q) + 252 0]2-(aq) -i> 2 1 -(~q) + S 4 o 62-(::..q)

U nrt 3 and 6: Chemistry Labor"atory Skills 21


S e t your wot·k o u t dearly.
~o tha t t.he exd.mine,. ean
u n der"'5tan d w h at. you are
calculati n~ at each s t e p -
d o not ju st .......nt e: down a
JUITib le o f n urnbet-s.
•
If "the tern.pet-ata..u-e rises,
t h e r-e.:t.ct.ion i~ exoth errnie
a n d so 61-/ is nesz;at Ne: i f rt
falls. 6H i s posi-t ive.
22
Content Guidance
CoJcul ~:tc :
(a) t h e nurnber o f rnolcs o f sod iurn t h iosu l fat.e in the m ea.n 'litre ( I)
(b) t h e number o f rnole-.s o f iodine lib er-a-t ed, and hence t h e number o f moles of
M IO, in 2SOc~. u5in.a your answer-to (a) (3)
(c;) 'th e molar n-tass of M I ~ u5ina your a n swer t.o (b) a n d the rna " of Ml~ u5ed ( I)
(d) ic:kan ti(y the a le m ant M in M IO:l U$in a your an 5~r to (c;) ( I)
(e) 1-fow .......,guld tho -tit.ret h:av-et been a lta rod i f t h e buratta h ad beon wash ed out w i t h
water and not with t h e sodium thiosu l fate solution? ( I)
An .:l lte t· n n trve experln'le nt p r ovides y ou with a soluUon of a n o x idi si n g agent a n d you
are asked to ffnd I ts con cen tratio n .
Knowl e-d ge c:.h ecdc. 1 3
2S.Oc.,.,"i o f a solu 'tion of h y d roa en p eroxide WAS pip et-ted into a. conical n a:sk.. Exce'S.:S
potas$iu""' iodic::lo a n d d iluto 5ulfuric .;u:id were added ;.n d -tha libar .artctd iodin e thr;,t.ctd a a a inst
0.111 mol dm- 3 sodium thiosu l fate solution.
T h e mean t1t.re was 26.4 Scrn 3 •
T h e equ ations for the react ions a r·e:
H 2~(aq) + 2 H +(aq) + 2 1-(aq) ~ l~(aq) + 2 H~O(aQ)
ll,(aq) + 252~2- (aq) ~ 21- (aq ) + s ... o,2- (aq)
Calculat.e;
(a) "'th e nurnber o( moles of sodium t hiosulfat.e in the m ean t itre ( I)
(b) the nurnber o( moles of iod ine. and h enc:e the num ber o( m o les o( h ydroae n
peroxide, in 2 5 .0 e.,....., (2)
(c) the eoneent.ra:tion o f the hyd~n per'OXide solution in mo l dm-~ usin~: your ansvve,. to (b) ( I)
(d) the volu me o f oxyaen 12as libet""at ed wher"'' I .O Odm~ o f this solution deeomposes: ( I)
2H,O,(aq) -+ 2H20(I) _,. 0,(11)
I mol of a ,aas occupies 24 d rn:l under "these cond ition s of temperature and p ressure.
Enthalpy change experiments
The keys to t h e calcu l ations a r e:
• t he heat change = mass of solullon x 4. 18 x 6T
• th nth 1 h n ... L.l _ h eat c h a n ge
e e a PY c a ge .......-. - * number or rnotes teacted
There a r e t w o t y p es o r experi ment .
( I ) Estima tio n of l!t.J.I of a s ingle r eaction. A t ypi ca l m a r k a llocation I s :
A acording volu r"'"''q c a n d t:o rnpo r;at:uros '2 rnl')r k e
Drawi n g a nd lnt:c;trpra cl n a g raph 3 o r 4 m a r· k£
A c c uracy 4 or S m a r·k£
Ca l c uiACi on 3 o,. 4 m a rks
Comme n t: I rna rk
(2) Esti matio n of 6.// for t wo t·cnctlon.:s and the usc of t l oss•.s law to calcu lnt e 6 .11 of u
thi r d .-eacuon . The m a r k al l oca tio n fo.- the two e x per i m e nts I s:
Ede><:Cel A S/A 2 ChEHY'Ii stry
 Unit 3

Reco rd i ng masses and t:ernperat:u r e s 2 marka each

/l.T accuracy 2 marka eac-h
Cal cu l at:lon o~ /l.H 2 marka eac-h
Final cal c u l at:lon usi ng H ess•s l aw 2 marka

Experimental methods K n owlc.dgt'> ch""'ck 14

There arc three different techniques - they all usc a plastic (expanded polystyrene) VVhy is a n expan ded
c up held In a g:lass beaker wHh a thermon1eter betng: used to sttr the rea c tants . polystyrene c u p used and
( I ) Mix measured amounts (volumes or- masses). Stir' and recorcL the statung and ncrt a akts:s bca.kcr?
n,nxltnum t cn,pernturcs. Thl5 tnethod Is used for rupld n ::uctlon:s, s u ch ns ncld/
base or acid/carbona t e .
(2.) Record the tempel'atuce or one solution lb r several minutes. then add the other
reagent and tnea.su re t he temperature overu peri od ofU tne. A gfi:tph o r temperature
usalnst tl n,e I s then plotted. This method I s used for slow reactions, such as mota I /
copper su lfate soh.atton. or t o measu r e the enth alpy ofsolutton of salts.
(3) Measure the tntu aJ temperature or one solution and add poruons or the o ther
solution at regular Intervals, rnoasurlnB tho temperature ouch un,o. A gruph o f
temperature agatn st vol u n'le added I s t h en plotted. This n1 et h od ts a l so used for
rapid reactions. such as acid/base reactions.

Errors In technique

•
•
•

•
Not u si n g the bottotn of tho n'lonl.scu.s to read vol utncs.
Failing to sur the tnl xture t h orough ly, and so not observi n g the
cor.-ect teJnpecatul"e.
Falling to road the tompcruturo to .sufOclc nL accuracy. You urc
..
advi sed to r ead all ten'lperat ures to an accun:.cy o f .a:O. l °C, so you
must be prepared to estimate It between g r aduations If you ace
s u pplied wtth a Lhermotnetefcallbrated. to o.z• c. ·rhe temperatu re
In the diagram I s 3,-:'L 3°C.
• ca r eless addition of solid . If a gas IS e volved, as In the reac tion
between a carbonate and. an actd. c al"e must be taKen t o add the
solid In .stnu ll porllon5 to prevent any .soluuon frothing up out o f
t h e plastic cup.

Errors In recording
• PatllnQ: to record all masses t o 0.0 1 Q. For example. a mass of 1 2.~Q rnust not be
recorded as t2. 3g.
• Failtng to r ecot·d ten1perature t o I decimal place. Y ou mus t r ecord a ll temperatures
to O.I°C,
• YOu must record t tme.s to un accuracy or a t Jeust 1 minute.

Errors tn graph plotting

• A sen s ible scale must be chosen. M ake sure that at least half of each axis Is used
t'or t h e readings. Do noc stan the temperature axis at zero deg:rees.
• check that you have p l otted each polnl accurat e ly.
• Do not forget to l abel both axes.

U nrt 3 and 6: Chemistry Labor"atory Skills 23


A s sume that tho c:le n s;zy
of aJI aqueous solut.ions i s
I acrn-3. This rno~n s th ~t
the mass •s n u m e rically
equal to the volu me.
If you a r e asked l O Slive
your 011nsvva•· -to 1::!..1-1 -to 2
siaruficant fiaures, make
s ure th4t. you d o so and do
not aivcr it -to 3 o r rnoro.
• t:J../<1 will be negative I f the r eaction I s exothcrtntc (the tempcruture rl.scs) und post li ve
appropriat e numbe r
of sian ific ant. fiauroes is tha t.
of t h e number o f ~anifi c~ n t
fiaures •n the v a lu e of 6 T.
If lhi:!~> i~ l e ~~ than I 0 ° . ro,..
example a tcrm pefdtuna
c h anae of 7 .6°C. Sli ve your
answer -to 2 s.f. If i-t is over
I 00. f o r example a chanae
of 23:1" C. you sh o u ld aive
your ans wer t o 3 s.r.
24
Content Guidance
• Make sure that two best.. fit straight Hnes are drawn usrns a ruler. Do not join up t h e
points.
• extrapolate both lines backwards, so as t o be able to measu re a maxhnun"l a.T o r
the volun"lc required for ncut ralt.sauon - sec Knowledge checks 17 nnd l S .
Calc ulation
• The fir st step is to ca l cul~te the heat chan"e;
heat cha nse (ln JOules) = mass o r soluu on x spectnc heat capacity x a.r
heat cha nge I n kJ = heal change In )/1000
The specific heat capacity wHI a l ways be given. A comn"lon error is t o use the m ass
of a r-eagent and not the n"lass or sol ution tn your cal cu l ation - see Knowledge
check 15.
• The second step i s to ca l culate the number of rnoles reacted . For' a soltd this iS;
m ass
mo lar mass
For a solution It ts:
con centration • volume In drn3
• The thtr'd step ts to calculate b .H:
heat c hange tn KJ
6 14 - · -----c----~---C=-----~-----
numbcr o f n,olcs rcncttng
f f the reaction Is e n doth er mic ( the ten"lper~ture f a lls) .
It IS a comn1on er't·or to tgnore tile stg.n or b..H or to g:et ll wt'ons;c.
Comment on accuracy
You rnny be asked Lo com 1ncn t about whlch Is t he l east accurate piece o r cq urpn,cnt
- th is '\Vtll usually be t h e t h e rmo n"leter. For a the rmo m eter r eadi n g to O . l°C for each
reading, t h e ert'or for each readtns;r Is *o. 1•c. As two .-eadlflt~C:S were taken to measure
t:!t.T. tho porcontnge error Is ( 2 1,P
1 ) • 10096.
lncreasln" the voh.1me of soluti on con tal n l n " a reactant wil l inc r ease the heat
ptoduced. but wUI proporuonately tncrease the mass ofsoluuon that ts heated up. :so
I t will have n o effect on e..r and h ence on t .h c accuracy. Inc r easing the concen t r ation
of a sol ution o r t h e m ass or a solid will i n c rease the value of AT a nd h ence tncrease
the accu racy.
Knowledge c h eck JS an example o f a r apid roc.1ctlon u s ing the technique that Invo lves
meast.u-ing the tnltfal a nd fi n a l ten"lperatu r es .
Ede><:Cel AS/A2 ChEHY'Iistry
 Unit 3

K nowl edge <.h ec k I 5

VVhen 2.56~ of po"tassiurn carbonate. K2CO,. was carefu lly added t.o 2S.Ocrn, (an excess) of
2.0rT'Iold,.,-l hydr-ochloric a.c:id, -the ternpe •-:..-ture ro:se from 23.7°C -to 3 1.40C:
K2C03(:s) + 2J..~CI(aq) -t> 2KCI(aq) + C02_(&) + ~20(I)
A:s:su rnina tha:t -the :specific: h ea:t; c:~pacity o f the solu ·tion is "'1.18 J 8-1 oc-1, calculate:
(a) the heat enel""'lY transfer.-ed (I)
(b) the enthalpy ehanae. 0.1-/1 , s:iv ina you r answer to an AP't=)I"'p•-i&te number o f
s i a n ificarrt fi,guro s

Knowledge check 16 l:s an example of a Hc:s:s•.s l aw cal cuJallon.

K nowl edge c h eck 1 6

Potass.urn hydro.szencarbonat.e also reac"ts w im acids:
KHCO,(s) + H C I(aq) _, KCI(;>q) + CO,(sz) + H,O(I)
GM.an t.h at t h e e n thalpy chan,ao. ~~.fo r t.:hi:; I'"'Qac-tion is + 29kJ r-no l- 1 and u;;ina your answer
to KnOW"Iedae c:hec:k I S (b), draw a Hess's law d iaar-arn and calc ulate t:he vaJue o f O.H for the
reactio n :
2KHCO,(s) - > K,co,(s) + C=O,
.=,_,("'
sz)
"--+--'-
H..:.>o.O
= (;,;
I)_ _ _ _ _ __
Knowledge c h eck 17 rs ror a slow reactton.

•
K nowl edge c.h ec k 17
2S.OcrnlofO. S00Moldrn-'l eopper(t) :!lulf::a:te solution wa.s poured in-to a polystyrene e up and
iu temper.orture I'T"'tQ~red every rninuta for 3 rnin uws.
..
At the fourth rninu'te. 1.3 a (an excess) of zinc was added and the temperature measured for a
fu rther 6 m inutes:
Zn(s) + CuSO-.(aq) -Jo ZnSC>.,.(aq) + C u (s)
The l~oSUits a.rc shown below.

T i m e/min 0 2 3 s 6 7 8 9 10
T o rn pcr at: urc/°C 22.0 22.0 '2.2. 0 '2.2.0 2.9. 3 30.7 30.2 29.8 29. ... '2.9.0

(:t.) Dr:tw a a,. ph of tornpar=ttul-o on t h o y - axis na:linsrt tirna o n -tho x.o;u.cis. (I)
(b) Dr:tw ~ lin a o f bast fit from zoro to tho third rninuto. nnd .::.n othar from 'th e
s ixth t o t h e ten"t.h minute. Extrapolate the lines to the fourth minu"te and
c:al c u hrte the ertima:ted tel"'"'pera'lure r i se. (max. S)
(c) Calculate the heat. cha n£e, as!!:u m ina that the solution has a specific heat
capacity o f 4 . 18Jk,C 1 °C 1 and a de~ n si ty c f I szcrn-3. (I)
(d) l-len co c;o;llc:ulatCI t h o an-t.h.alpy c;;~naa to 2 s isz_nifican-t fiauras for tho I""O...ction,
szi vin~ a siszn and units with your answer. (3)
(e) What observation shOVIIs that. the z inc was in exeess? (I)
(f) Would doublina a ll quant.it.ies increase t.:he accuracy of your result? JustifY
you r ans.......ef": (2)

U nrt 3 and 6: Chemistry Labor"atory Skills

 Content Guidance

Knowledge check I S fs for s t eady addition of a reactant rn a rapid reaction.

Kn o w l e d~ e <.h ec:.lc. 18
Solutions o f n i t:.-ie aeid and sodiu m h y d roxide were a iiO'V'IIed to reaeh the same -temper'atu l"e o f
IS.0°C.
SO.Ocrnl o f -the nitric .:tcid w::as p ipc:rttod jn'tc:) .:t polysty1-ono c u p .,.nd ::a 2 .0 .,-,ol drn -3 solution o f
sodium hydroxide was added. w i"t:h st.in-inii;. in S.Ocm-3 portion s. The tempera"ture was not.ed
a fter eaeh addition.
The l"eaet.ion is:
HNO,(a"') + NaOH(a"') -+ NaNO,(a"') + H 10(1)
The r-esul"ts are shown below.

Volume o f' s IS ~0
~·
0 10 20 25 30 35
N aO H / cms
Temperacure/ °C 18 .0 19 .8 2.1.S 23.5 25. 0 2.6. 8 27. 2 2.7.0 2.6.7 2.6. 5

•
'-"'iume of N a 0H/crn11

\/'v~>e ,nyou have pl ~t.ed
tho poi nts, you rnu !;t.
draw two rtra.iaht hnes.
The hiRhest t emj:>er'a\.u l"'e
ro;achq:d is whorct they
tntersect.
(a) Use t:he w-aph to calculate C:t.T (or "the reaction and the volume of' sodiu m hydroxide
thAt ex.:let:ly neut:•-afi.ses the n i t.rie aeid. (7)
(b) Use you .- answe .- to (a) to calc u late the volu me in -the poly.styr"ene cup wken -the
nitnc acicl h ad jus't. boon n out.r~ l isoc:l. ( I)
(c) C.:::.lcul.::ata tho ho.::a't. chanao fo r tho nout.-.::alis:.rtio n o f tM n it rtc a.cid. ( I)
(d) Uso t h o volume c:.lcuL:ttod in (n) -to c::alcu ln-to t ho nurnbo.- o f moles o f sodiu,-,
hydroxide reQui red t.o neu"tralise the n itric acid. and hence the nufT'Iber of moles
of the aeid. ( I)
(e) Use you r- answer"'S to (c) and (d) t.O ealeu lat.e the enthal p y of neu t..-ali:sat.ion of
n itnc: ac:id . ( I)
(f) Is this .:::..s ac:c:ur-ato a ,-,Qtho d for find ina tho c:on c:ontr-a't.ion of ;;r,n .ac:.id c;ornparod
with a standard acid/base u~··~ra ;.:;t
~;~
o ~n ? _ _ _ _ _ _ _ _ _ _ _ _ __
c;:, ( I)

26 Ede><:Cel AS/ A2 ChEHY'Ii stry

 Unit 3

R.aad a nd r GCord: • do stir t h oroughly in t.harrnoch emist•-y axper irne n ts

• all rnc.sses t.o 0.01 g • only use con cordant titres (±0.2cml) w h en
• all volumes In t lt r atlons to 0 .05 cm3 calculat:Jna t h e mean tJtre
• a ll t.emPQratures to o. 1 •c don't leave the funnel in the top of the bur ette
Oos and don'ts: • don't add S"t<lrch t oo early in Iod ine titrations
• do ShaKe the flask thorou ghly whan making up a • don't forgQt a sign in t h Q :oanswQr of ~H valuQS (minus
solution iftha temperatu re rose and positive i f it rell)

Activity D: Preparation
rn al l prepa r ation s you w i ll be asked to wor k out th e per centage y i eld . T h is will scor e
2 or,:) or the 12 •nai"I<S In the assessment.
T h o O"lCth od I.S:
( I) work out the n 'lola r n 'lass of the rea<;ta n t th:;tt you measured out a n d of t he p r oduct . Rem e m ber t hat t he
( 2 ) use the expr ession moles tnass to ca lc~,..tate the nu n "lber of moles of react.a n t . pei""Cenu~e yield is not
molar mass m a..ss of produ ct o~
( 3 ) I f t h e reactant and p t·oduct are 1n a 1 : 1 r a.tlo In t ho eq u ation. the t h eor e tical m ass of reactan 't )( 1 .....~.
n 'loles o f product - tno l es of reac t ant.
( 4 ) T'h e ore ttc.a l mass of product = t l1eoret1ca1 motes,... molar nlass.
(
& )
96
ield _ actual mass o f product )(
10096
y t h eoretica l n 'lass of p r oduct

• Inorganic preparations
You w ill a l w.2ys b e ·told
..
You will be t·equir ed to p 1·epare ei ther a sin'lple sa l t such as copper(u) sulfat e or n ickel (n)
-th e f o rmu la of t h e salt.
sulf'ate. or a doubl e sa l t such as a1nmontu1n lron(u) sui tate. vou will be given detailed
ineludina the n u mber or
1nstru c tlons. A n y sal t you prepare wi ll cont a i n water of cryst n l lts.atton.
m olcc::u los o f water of
c:rystallls.abon .
P reparation of a simp le sa l t
T h e solid reacta n t Js added a lit tle at a tJ n 'te t o a know n volume o f ilCid , w h ich h as
been gently heated.
W h en t here t.s a s light excess of solid. the soiLtllon t.s Oltered I n t o an cvaporal lng bttsln
a n d t h e fl ltrate evaporated unti l about. ha l f of i t s Initia l volume r e m .a Jns.
The solution ts cooled overnight and the c ryst als de'ted by press11,Q: betwee11 sheets of
fil t er papet·. ·r he crystals nre then wclgh ed.
A typica l mark scheme i s:

R ecor d ina t:h e m asses I o r 2 m a rks

O b ser vatio ns a nd com m e ncs o n cechn tque 3 o r 4 m ark s
Oesc r t pclon o ~ 't:h e appearance o 'r p roduc't: 2 marks
C a l c ulact o n o 'r per'cent:aae yiel d 2 marks
V a lue o~ % yie l d 2 markS If >SO%
I mark If bot.woon •9 and '2.5"
Com m o nt: a a t:o w hy ylold Is < I 0 0 % I mark

U nrt 3 and 6: Chemistry Laboratory Skills 27


Kn<:>wledgc:: c:_h oc.lcc 1 9
ClSic:ula:tc the y ield o f
an experin-.en t where
5.67 a o f l"'iekel s ulfate.
N iS0 ... 6 ..... 20, wAs n-.~do
from 2..24 ~ of nickel( I()
oxide, N iO.
• Mass of hydrated copper(tl) sultat.e
Exan "'anE>r c:i
Y o u m u s l d e scri be 'll"'e
c:olou r o::~ n d s h a p o o f t ho
crystaJs.
Content Guidance
Errors In technique
• Not having t h e acid sol ution h ot e n oug h .
• Actdlng the solid too fast so that n froths up and overnows.
• evaporating the solution t oo rar so t hat some anhydrous salt IS formed. o r not far
enough so that too much product rc.1na 1ns tn solution.
Errors In recording
• All the masses tnust be given to 2 elect mal places.
• The descrtpuon or the cryst als mus t Inc lude thetr col our and their s hape. for
lnstanc.e green und needle o r dlomond shaped.
Knowl edRe c:.h ec:.lc. 20
U sina a rY'Ieasu rina cylinder. 25cm3 or I.O rY'IOi d •n-3 sulfuric acid was transferred to a beaker
:1nd tho solution W;11"lTiod. Por-t ions o f c:.oppcr(ll) c:ocido wore ~ddod with s-tirrina unt il t ho base
was in excess.
T h e h ot :roolution was tittered and the :roolution ev'apor ated to half it.'S volume. The solution
wa.5 l eft t.o cool. T he cr-ystals fol""'"l"'l'ed wer-e dr-ied and weiaked in a p.-e-wei£:hed weianinil.
bottlo.
Masc of c:ont:aln~ew + hydr~~tod '29. 6 6 B
copper(U) sultat:e
Mas s of empty c:ont.alner 24. 6Sa
(a) VVhat was observed as "the copper(n) oxide was added?
(b) VVhat sho........-ed that the coppe •~ oxide was i n excess?
s .o 1 a
(2)
( I)
(Q VVhy must the solution not. be evaporated "tO drynessl ( I)
(d) Oesc.ribe the appearance of the c:.ryrtaJs.. (2)
(e) C a lculate the mass of CuSO,...SH 2 0 (M ,.= 2.49.6) tha-t could be made from
2S em3 o f I .OrY'Ioldn-.- , sulfuf"ic add. (2)
(f) Calculate the percentaae yield o-f the preparation. (max. 3)
(a) V\lhy i s the y ield l ess t:h an ~
10
::..::
0;,:% 1 _ _ _ _ _ _ _ _ _ _ _ _ __
;::;. (2)
P repa r ati o n o f a d o ubl e sa lt
The most likely double salt to be used I s hydrated ammon lun, lron(u) su lfate.
The preparation I s In three steps. and the details tbr each will be Q:lven Clear'ly.
( I ) Prcparauon of a solutiOn of Jron( u) sulfate. A known mass of Iron flllng:s IS
reacted with a sllght excess of h ot dllutc sulfuric acid. Any unrcactod Iron Is
filtered off.
(2) Preparnuon ofat1 amnlOJllum suifateso/uuon. Di l ute ammonta IS added tn pol'tJons
to dlluto sulfuric acid unul tho solution Is ulk.ollnc to litmus. The excess an,monl.o
Is then boiled off.
(3) MbdllSf the solutions ana canylt1Sil out patY:/al evaporation. The two soluUons are rntxed
1n a. beuker and the mixture carefully evaporated unu1 the volume hus halved. It ts
then left: to cool and the crystals are filtered . dried a nd weighed.
Ede><:Cel AS/A2 ChEHY'IIstry
 Unit 3

A typical mark scheme ts:

Wal,ghlng tho Iron and t:ho p r o duct: 2 rnnrkc

Obsorvat:lo-n• and cornrnqon t:s Q n 3 or 4 rn;:.rk •
c:eehnlq u e
Appearance o r c:rysc:als 2 marks
Calculati on o f percent:age yiel d 2 mark s
Va lue o f X yield 2 markS If> 50%
I tf boc.ween 49 a n d 2S%
C:orn"'en t as ~o w hy yield •• <100% I mark

Errors In technique
• Not havtng the acfd so luuon hot enough for the reactton with Iron.
• Adding the solid too qu ick l y so thn t It fro ths up <=tnd overflows.
• Not sttrrtnQ" the aCid soh.a tton when addfnQ an1mo-nta.
• Evaporallng the .soluuon coo tar. so that some anhydrou s salt Is formed.

Errors In recording
• All the n "'asses mus t be given to 2 decimal p laces.
To sc:.on;t full rn ~rks fo,..
• The description or the crysta l s must tnc lucte their colo\.ar and thei r shape, for yield ~nake sure t.hat. for
Inst ance g:reen and need le shaped or d iamond shaped.
~ s inale s~ lt, you rn.a.ka a-t
Kuowl e d ge ~ h ~~ k 21 least 1.7Sa ofprodvc;-t

• 25 c:.m3 of dilute sul furic: acid was placed in a beakel"' and heated -to just. below boili nsr. 2.75 a o f
i ron w::ts .::added i n sn-1nll portion s, .::and .::a.ftc,.. anct, .2ddition a p lua of cotton wool W:t.S p l ~cad in
the n eck of the flask. F='inally an extra 3 c:_m3 o( add was added and the solu-tion fil'tel"'ed.
25 c:~ of dilvte sutfuric:. acid was added to a beaker and 30cm3 of ammonia solu'tion added and
ar-arn o f narti nll mat,er;al
and f o ,.. t h o double sal t n t
least 3.S a per araiT"' ofu-on.

sti,.red. Ful""thel"' Sc~ pol""tions o f ammonia wer-e then added until a dr"Op o f t:he solution (...emoved
vvrth A &l._ss I""'d) -tv,....,....od I"'Qc;lli trnvs b l vo. Tho solution w~s boilod 1:1:> •-ornO'VCII etxcetSS aiTIITIO n ~.
Tho two solutions .........,gt"'CJ l"nixetd .:and -thon boilod unt il t h o vo l un-~o h .:ad b<oon l"'ctduc:od by hal f.
l't was left to cool and the cr-ys'tals tha't (o,..med wel"'e filtel"'ed off. dr1ed and weiahed. They
weianed I 5.2a,.
(a) Why mun ·the ir"'n not be added all al onc:.e? (I)
(b) Why wa.5 a plu ,2 o f c:ot.-ton wool placed in the neck of the Oa5k? (I)
(c:) tn the proepar"&t.ion of the second solu t ion, was the ammonia solution in excess?
Justi fy )"QUI- ::lnswor;
(d) Describe t h o .::appo:u-.:..nco o f the::. cryst:tls. (2)
(o) CAlculate the thoorctic.:..l y ield of AITI,oniuiTI iron(u) :su l f.::atc,
(NI-t4 n_so.... J:os0 4.6~2o (ITiol nr IT"'nss = 392.0a,ol-')•
.::assu~T~ina th~t I mol o f iron p1-oducas I mol o f 'tho hydr::rtad dou ble s~ lt. (2)
Yov: IT"'Vr t do5Crib9 t;ho
(f) C.alculo.t.c the por-c:cntA&C y ield of product. (I) colour and s h ape of t:he
(a) Why i s the y ield lcs:s t h .::a.n ~
I0
=-:
09Q
..:..:.:__ _ _ _ _ _ _ _ _ _ _ __ (2) crys-tl:lfs.

Organic preparations
Ful l details of the proceoure wil l be gtven and they should be followed carefu lly .

U nrt 3 and 6: Chemistry Labor"atory Skills 29

 Content Guidance

Tec hnique
• You must know how to set up apparatus for distillation while addJng reagent, and
for dtstfltatton .
• Make s ute that the water" nows Into the condenset at the bottom and o ut at the t op.
• check that all the Joints are sound and that they will not leak.
• Check that a thermometer, if fitted, is opposite the entrance of the condenser.

Oxidation of a primary or seconda1· y alcohol

A Known volume or the alcohol ts dissolved rna solu[lon of potassium diChl'omate(v•).
very cnrcfully, :sontc concentruted sulfuric o.cld I s added to some water In a flas k.
Thi s Is then connected to distillation apparatus that is adapted for the addition of a
r eag-ent and brought to the boll.

Eth:lnol + potuslurn dlchr"om:lto{va) solutton

Water out

•
Sulfu nc 2cld
I
W:l.tor ln

rnus t b e p r e p a r ed
t.o draw di ~ral'ns of
leo 2nd
app:u-;~:tu s , such .:1s th is ono , Wllter
in "the U n 1t 2. pap e r.

The alcohol and potassium dlch i"Otnate(va) solution is then added fron-. the tnp funnel
a few drops at a tln"'e.
J'\ prrmary alcohol Is oxldtsed 10 an aldehyde, whtch dlsuts over as l l Is formed anc::t 1.s
collected In a flask s urrounded by Iced woter:
C H 3CH :,aOH + 101 ~ CH3CHO + H:aO

If heated under reflux, a prlmnry alcohol wou ld be oxldlsed to a carboxyllc acid !

C H 3C H:::~ OH + 2[01 ~ C H 3COOH +- H:aO

30 Ede><:Cel AS/ A2 ChEHY'Ii stry

 Unit 3

When heated under reflux with the oxidising agent a secon da r y alcohol Js oxldlsed to
a ketone. The apparatus Is then chanQed to dlsti l lat1on and the l<etone is dtstt l le<l off
and collec ted In a l'lask:

Aldehydes and ketones can be t ested for by addtng a soluuon or

2,4 - d l nltrophonylhydrazl ne. They glvo a yellow or orange precipi tate.
Aldehydes can be tested for by add in" to;
• Tollens· reaQ:ent, whiCh gtves a sliver' mltror on warmtng
• Fohllng•s (or Bonodlct's) sol ution, wh ich g;lvos u 1·cd proclpltntc on warming.
carboxylic actds react with sod t um carbonate (or hYdrog-encarbon ate) to evolve a gas
whiCh turns H1newater cloudy.
A typica l mark schenl.e Is:

Ob•orvat-lon o ,- t;q,st- o n p r o duc t; 2 IT'I ~rk.c

Ob eq, rv at:"lo n t~ d u rin g o xldat;I Q n I IT'I<llt""k
D ot~c r1p t;1Q n o ,- pro duc t: I or 2 IT'I ark~:
B o ili n g temp4 r at:u r-e o~ pro d uct: 2 IT'I<Iot""~*

D iscu ssion o f t;echnlque 3 or 4 IT'Iarks

M od l flc a c:lo n o f apparat:·u s 2 or 3 IT'Iarks"t

• •Only i f tho product is rodistillod

t-Onl y when a primary alcohol is used (s;ee part. (a) below) ..
Kno wl c dgg c:h c::c k 22
Ethanol w::tos oxidi=:;od as do't.::ailod :.bovo. T h o produc-t was 'tasted by :::.ddin a SOI"T"IO
2.4- d init.rophenylhydrazine solution.
(a) What was obsel""\.\'ed on addition of 2.4-c:hnit.rophenylhydra.zine solution? (2)
(b) Why was the sulf"uric acid added to t.h e wa"t.er. and not. the water-to t.he ac•d? (I)
(c;) What colour chanae took p lac:e durina the oxidation? (2)
(d) D escribe the product collec:-t.ed. (I)
(e) V\lhy is it necesS-ary to h ave a vent on the adapter connected "to 'the collactina ve55el7 (I)
(f) V\lhy I"T"IUst "the et.h a n oVdichromate I"T"Iixtvre be added a f"ew drops at a time? (2)
(~ How would thoa apparaws be adapt.ed to pr-epare etha.noic acid from ethanol? (2)

D e hydra cio n o f a n alcoh o l

A n alcohol. such as cyclohexanol, can be dehydrated usfng concen trated p h osphoric
actd, ptoductn" an alkene.

0
T h e acid and the alcohol are m 1xed and the cycloalkene Is distilled off.
-+- H,O

U nrt 3 and 6: Chemistry Labor"atory Skills 31

 Content Guidance

Wator ln

must be prepared
t.o dr""aw d id.2r"al"r"'S of
app;ar~tus, S~.~c;:h .;as thi$ o n e ,
tn the Un1t I paper. The proelucl can then be tested wtlh br•omlne wat er.

Kuowl c:>dg., c:h c-c:lc 2:1

So.,-,o c:onco~'tod phosphor ic acid, ~ ITIO:.t'liurad volu.,-,o o f cyd ohox::u"''CCI a n d : l few anti ..

•
bun-1pina Qranules are placed in a flask which is then attach ed t.o dist:illation apparatus •
T h e Oask is ~rrned and a mixt.ure of wat.e•· and cyclohexene distils off a.nd is collec-ted.
The rnixt.u l"'e is poured in"tO a separa:ti na funnel and the lo........er aqueous layer d iscarded. -,...e
upper laya•- is r u n into a flask a n d lumps o f c~ l ciuiTI c h londo added. Aftcar a fow rninutos, 'tho
cydohexene is p oured off and distilled.
(a) VVha"t is obse~ when some of t.h e cycloh exene is sha.ken wit.h bromine water? W r it.e
the equ ation for the reacotion. (3)
(b) Why is the c:yelohe.xene in t.he u pper"laye•• in the separ""at.ina funnel? ( I)
(c:) What is the funet:ion o f the c:alc:iu m c:hlor""ide? ( I)
(d) Why mus1: the ther"mome"ter" bulb be p lac:ed opposite the mouth of the condenser'? ( I)

• Make su r"e that you r yield Is > 50516. • Make sure tha-t there are no leaks in Quickflt
;~.ppoar;nus.
• When crystallis ing a salt. from a solution do not
evaporate to d ryn ess. • R.Qcon:::l t h G colour b QTor G :Oillnd : rftg,r in a tQSt To r an
R.GtmG~ombG~orto r ocord ;;:all maSSQS t o 0.0 I g. o~nlc pr"''duct.
• Record the sh:tpe ;).n d colo ur ofth 4il salt: produ ct.

Ede><:Cel A S/A2 ChEHY'Iistry

 Unit 6

Unit 6
Activity B: Qualitative observation
Organic subst:ances
ln t:roduct:lo n
rt I s lmpo t·tant to read the student brief carefully. H i nts mny be given such as:
• each orga nic compound conta ins o n ly o n e fu n ctio na l group
• u'e nu 1nbet or carbon atoms that •no tecu les or each cor.npound contains and
w h et h er It t s a br<lnch cd or a s trulght- chafn corn.pound
• t h e fact that one unknown m ay b e oxidlsed, reduc.ed or hydrolysed t o anothe r of
the unknown or unknowns
You wHI always be g i ven tho quantities o f both tho unknown nnd t h o tes t reagent and
full det a tls o f h ow t o car-ry out the test, so you do n o t n eed to l earn these. Exa.tniner t.•p
Maka sur-o th.::.t you c::an
Althoug.h t h e matn part or the task wiH be about s ubstances met In unit 4, quesuons 1nterpre1; mass. inf"rared
will b e asked ubout ulkoncs, aJcohol .s or possibly halogonoal kancs, so these mus t and NMR.speet.r"a befor'e
also be r evised before the prac tical assessl'ne nt. )"'0\.1 d o t ho aSSQSSIT\Ont.

•
M ake sul'e that you know tt1e difference between dis pl ayed rormu lae (a ll the a t oms
and bonds n"l.us t be s hown) , str u ctura l forn"lulac (un unan"lblguous fonnula s h o wing
each group sepa r ately) a nd s ke1et:a1 forn"lu l ae.
..
.... .... ....
H- t- jT- t- t-1-< CH ~g CH.,CH~
~ 8 ~ ~
Dtspfayod Stru ctur:.J Skelot:al

M a k e sure th4lt your deduct ions are loQical . T h e deduction from a postttve Iodofo rm
t est ts not tha t the unknown ts one o r ethanal . a methyl k e t one or an a lcoh ol wtth a
CJo1.3CJoi (O I~t ) s•·oup If y ou have already shown that an unknown I s a kot o no.

T h e t.• nknow n s that you could be asked to Identify are:

• alkenes
• alcohols
• halog:en oal kanes (n ot v e ry likely)
• aldehydes and ketones
Examtner t:1
• carboxylic <tC ids
Make SUI"'e that yo u know
• carboxylic ac id d e rlvtltlves ( n o t very likely)
tho to.st for ~ ldahydos ::and
POSSible observations mai'I<S are s hown Wlth a ...-: ketones.

U nrt 3 and 6: Chemistry Labor"atory S kills 33

 Content Guidance

A typic al mark s cheme I s:

Draw "the skeletal fo rmula Obscrvat:ions B or 9 marks
of ,.,.,c:rthylprop:snnl.
Analy sic o~ spoc;t: ra 2 or 3 marks
l d o nt:ifica t:io n o~ unknownc 2 or 3 marks
Con'lln'll ctnt: on produc t o'f r ·eactlon I m3rk

P ossi ble t es t s
Combustion
T est: Obscrvat:lons ln'fcrc nccs
Burn n fow drops. on • • I t burns with n cfe<'llr n o n -s.moky
name V'
• l-ow c;.rbon-to-hydrogon
ratiO
eruelbl e lid
• I t burns with a smoky flame V' • •-ugh car bon-to-hydrogen
ratiO

Solubility In water and pH test

T est: Observat:lons l nfe renc.es
Add t:o wat:e•~
• Either cwo layers fof"tn V' • Eicher no OH group: or If an
alcohol or acid It has a hlah molar
n·.-:11s5 (ace l o::uc f ou •· carbon a.t. OIT"'S)
• Or lt. dlssolve..s fully V' • Forms hydroa:en bonds Wlt:h
wntcu·, &o has :.n O H group
Add litmus. or
universal I ndicat-or (U I) • U tmus paper (or Ul
solution) aoes r.ed .,;
• It: I s an acid
liC!uid i~ m ix ed with
water. • Ul solu tion goes green .,; • I t Is a neutral substance (not: an acJd)

Test for alkenes

T est: Observations I nf'c r cnccs
Add 5ome bromine w:.t:or to Brown bromine wa.tor goos C•C group p•·osont
t:he unknown - stopper tl"te colourl ess. V' and two layef"s
toct tubo and shako carofu fly aro formod .,;

Tests (or halogenoalkanes

T ost: Obso r-vadons I nf'oronccs
Shnko a fow dropc o f 'tho T wo layer• form ....
unknown with water
Add a few drops or ethanol and
aqueous sliver nlt.ra.te a.nd dllut.e
•
•
White preelplau:e .,;
C •·onrn procfpltnto V'
•
•
.. contains
IC contains
ac Cl group
•a CC -Br group
nl'trle acid - - stand the test 'tube
In a bea.ker of hot. water
• Yellow prec1 p i tate V' • IC contcalns - 1 group

Add 4 drops of et.hanol and

•• Whl'tct prctclpltaur .,;
thon 2crnl o f dlluto sodlun-l c .· earn preclplt.ate .,;
hydroXIde- st:and the test: t:ube
In a boakor of hot wa"tor f or S
• Yellow pr"eclplt:ate V'
• l t. cont:alns a c C l group
• It con tains a C - B r group
• It conu1n.s a C -1 group

m i nutes: then add excesc nlt,.IC

ac:ld followed by aq~o1eous sliver
nitrate

Ede><:Ce l AS/ A2 C hEHY'Ii stry

 Unit 6

Tesc O b s ervations I nfer·enc:es

A dd concencra~d •odi um
h ydroxl do In oth a n ol - f h . ~ho
• Brown bromi ne 8:0E!S
colour-loss .....
• H - hatoaen ellmlnaced
formi n g an a l kon o
test tube with a delt'Very tube
\3n d wa.rm sen d y , passing ')n y aas
evol v e d throu gh a li t tl e bromi ne
w acer

The tdenuly or lhe halogen In lhe prectpllate formed with s liver nttrate can be
connrmed by adding arnmonta solution .

Obse r vation l n f'o f"onco

P rocf p l t .n t:o d i ssol ves In d l luto nmmonla. .....
P r ocl p l t .a t:e fn sol u b lo In d l lut:o b u t soluble I n
concentrated ammoni a V'
The u n k n o wn
T h o unkn own ..•• •• chlor o;<tl kan e
b ro m oalkan o
Tho ~qu:;rtiQ n$ for tho
action of' aqueous S tiver
ni·t l'""tlte ar-e:
P recipi tate I nsol ubl e In conce ntrated
a mrno n l<t V'
T he Ul'\known
•• an IOdoa.Jkane R..- X + I-I20 _... ROl-l +-
1-1... + x- ;an d
Test for aldehydes and ketones x- + As:.... ~ AaX
T h ese cont a tn the C=O grou p.
Knowl e d ge c h ock 2!;;.
Tesc Observaclons l nf'er·ences D r.aw tho rt•·uc:tur:a.J
Ad d a f e w d ro p s A y ell ow or orange It I S an ald ehyde or a k e cone formula o f the product of
of a sol ucton of prec l pltaee .,.

• 2,4 •dlnlt:rophenyl h ydnu.tne

Tests to d1stinguish between an aldehyde and a ketone

and propanono.
..
Tesc O b servaclon s I nferences
Add a few drops of che •• Elt.her red precl plcat.e V' • l t. IS an a l dehyd e
unk n own t:o som o F ohlln g'a (or
Benedi ct's) sol ut.l on and waf"m
O r t h o b l uo col our r oma.lns V' • It l it a koton o*

Add a f e w d ro p s o f che • E lt.her sliver mlrt"Of" rorrned V' • It Is an a l dehyde

u n k n own c.o Tollen•' reaa:enc.
(s-oo b e l o w ) and warm
• O r solution stay• col ourl oslt .;' • ft. I s a kecone*

Add a. (ow dro p s o f t h o

unknown to acidified
• E tth or o r ang e solu t i on g oo•
aree n ..,...
• It I s an a l d e h y d e*

p o c.ascl um d l c hro mnto(v•)

solut:lon
• O r solutio n stays o •·a n go V' • It: l it a koton o*

A dd a few d rops o f the

u n k n own c.o $Ci cl tftecl
• E lthe.r purpl e solutton
d e col ourtsed V'
• l c. I s an a l dehyd e•

potassi u m manganate (vu) • O f" solu clon stays p u1• p l e V' • t c. I s a ketone*
s-ol ution and w arm

•This i nfe...enee ean o n l y be made i f the s u bsta.nc:e has already been shown t.o be a c:arbo nyl
c o m pound .
Ex-a m i n o r t:ip
Tollens· reat;(enl 1.s made by adding: aqueous sodturn hydroxide drop by drop to Remem ber that primary
aqueous s liver n itrate unti l a grey prec tpltato J:s formed. Tho clea r liquid above the alcoh ols c:an be oxidised 1.0
precipitate (t h e s upe r n ata n t liqu i d) is pour ed o ff and the precipitate dissolv e d In the aldohyclos and soc:on d;ary
1n 1n1mun1 ofdll ule a •n•nonta . alcoh ols to ketones,

U n rt 3 and 6: Chemistry Labor"atory S ki lls 35


Which of the followina
w ill nof: aivc A proc ipi1:~
of iodoform when alk a lin e
iodine is added: e t h a n a l.
propan..2 ..ol, prop.:tn• l oool,
but.an-2-one?
· ~~<he
~
obs.erv.!t-tion is bubbles
(fizzina/effervescenc:9). not.
t.ha"t a aas is evolved.
Content Guidance
The Iodoform test
This I s u r eaction between an o rganic alcoho l or c arbonyl con~pound and a sol ution
oftodt n e and sod ium hyd r o xide . T h e mtxture f s t h e n allowed to stand.
Observa.clon P revtous test: I nferences
Pale yellow prec:lp tc:ace
(of Iodoform*) V
• A prec:lplt.ate W1<h
2 ,.,. - dlnlu·ophonylhydraz.lno -
• It c:oncal ns aCH -aC
group
0
showtna It to be a carbonyl
compound
• A r ed pl""e:C:Iplcate w'lt..h Fe.hllng·.s
(or Bonodh:t:' $) .-olucton o r
• It I S ethanal
a sliver mirror with Tollens'
reaaent:- showlna It: t.o be an
aldohydo
• St.eamy fu•-nes With P C i s or
othor tos t - showing I t to bo
• It c:ont.alns t.he
C t-I.,C I-f(OI-I) group, for
an alcohol (see below) exampl e propan-2-ol
*'Iodof orm's systemat.i c name i s triiodornetha n e . C H I"l •
Tests (or OH group in alcohols and carboxylic acids
Test: Observations I nfe r ences
Add a small piece of sodium • B1.1bblos evolved .,. • It:. cont:alns an O H aro'-•P
to tho unknown In nn
evaporattna basin
• Sodium dlsappe~u·s or a
whlt:e solid forms .,.
nnd so I s: i:'ln alcohol or n
carboxylic ac:ld
Add solid pho•phorus(v)
chlorldo nnd tost nny gns
• St.enrny f\.1rnoe evolved .., • l t. cont.atns an O H a:ro'-•P
nnd so 15 nn alcohol or n
evolved: e l t:her wtt.h a a•ass
rod dlppod In con contratod • Whlto crnoko forrnod
..,. carboxylic: ac:td
ammonaa: or with datnp blue
llt:rnuc p<tpf;tr
• L tc.mus aoe.s red .,.
To distinguish an acid (rom an alcohol
Teet: Obcervat:ions lnfQ. r e n cec
Add t:he \.tnknown to a s:oh..tt..lon • F-Izzing V • l eIS a carboxyli c acid
o f sodium carbonat;e or sodiu m
hydrog.encarbonac;e and c;est. any
• Gas evolved turns
llmowac.er c::I01.1dy V
gas ovol vod with ll1nowator
Add bluo litmus (or unl vors:\1
lndtc:ac-or) t o a solut:l on of the
• L lt1-nus goo~~: rod V • I t Is a c.11rboxyll c acid
unknown
Add sofTie echanol (or other
alcohol) and a few drops of
c:oncencrac.ed sulfuric ac:ld co t:he
unknown a.nd wa.•·m
Then pour tnt.o a beaker conca1n1na • 1=-1 :z:.z1 n a .., • l t.. h a carbo xyli c ac:ld (and
somo sodium carboni:lt·O solution
and c:aut..l ously smell t.he product.
• Smolls of gfuo/frul ty
smell V
nn ost.ae· I s for!Tlod)
Ede><:Cel AS/ A2 ChEHY'Ii stry
 Unit 6

To distinguish an alcohol (tom a carboxy lic acid

Obs e rvat'to n s I nfe ren ces
Add some et.hanolc: ac:td and a few
d r ops of c o n c:ontr;t.ted sulfur ic 3 Cid
to the unknown and warm.
Pour tnco a beaker c:onta t ntna
11ome sodiu m ca.rbonat e solu tion - Ftz:z.t na: ......
Smoll.s o f g lu e/f ru i ty - lt. I s an alc ohol (a.nd an
octor 15 f oriTiod )
E x~ mino r t-i p
A substance that has an
a nd c auaou s ly smell t.he prod ..•ct.
Warm che unknown aent:l y wtch
:..cldlflod potassi um dtch ro rn ato(v•)
s o l ut.to n
- smell ,......
O ranae sotudon aoes
groon ..,... - l t. I s a primary or
aocondnry alc.ohol*

....T h is i nfer ence can o n l y be made i f it. h as been shown t.hat. t.he u n k n ovvn cont.ains a n OH aroup.
0 1-1 &ro up, fo ,-.f'T'tS a.n e.ste.-
wit h e thanoic; acid bvt
d o es n o t cha n ae t he colour
o -f :u: idifiod pota ssium
dlchrornate(vl), mus~ be a
Thi s Is because a l dehydes a l so tur n acidi fied dichr"'mate(\1'1) ~ ~. 'tertia"Y a lcoh o l.

Tests (or acid chlorides

--
l ese: Observat:lons
A dd the u nknown t:o some water I n a t.est tube St:ea.my fumes .,...
Then a.dd dllu t.e nitric a c id and a queous sliver nlt.rat:e W hlt:e p r ecl plt:9 t:e V
Add t:he u n kn o wn $ O m e et:hano l a n d t:.hen po~o1r l n t:o
~ Ft· utty/gl u o *"' • II V
a bea.ker containi ng aqu eou s sodlutTl carbonllte
C arefully smell t.he beaker'$ concenu:

• Spec era
Mass spectra
..
vou may be Q tven a mass spectru m to help tdent U'Y t he unknow n. T'he nve values to
l ook for nrc:
• t h e la r g:est value ts due t o t h e m olecular ron. M•. .ttn d correspon ds to the relative
molecula•· mass or the compou n d
• n peak at ( M - 15) or tl t 15 due t o t h e p resen ce of a C I-t~ group In t h e m ole c ule
• a p eak at ( M - 29) or at 29 due t o enh e r a C~ l-1 0 o r a C H O g r oup i n t h e m olecule
• a peal< at ( M - 4 !lo) or at 43 due t o a C.:,H 7 gz-oup In t h e mol e c u l e
• a peak at (M - 4~) oz- a t 4~ d u e to a COOH s_z-ou p tn t he O'lOtecu le

Infrared spectra
Y ou w i l l be allowed to use t h e Edexce/ dat a booklet during the assessm e nt. b ut n ote
that It states that t h e C = O absor ption I n k eto n es I s I n the rang:e 1680- 700cm-•. T h t s
Js w r ong becau se on ly aron,au c k etones fall Jn th i S z-a n ge. AHphallc ketones a r e tn the
t·a n go 17 10..- 1720cn 'l- ' and a liph a tic ald e h ydes I n the range J720.- 1730c rn - •.
Look out for absor p tto n s i n t he ra n ge: E x •miino r- t:ip
• 17 10-1730cm- ' c aused by t h e C=O Q:rou p t n aldehydes, k etOI'\es and c a r boxylic T h e h)"droa en- bonded
actds 0-H a b soq :."tion i s very
• 173S- 17SO c m - 1 caused by t h e c - o g r oup in ester s broad nnd it is difficul-t:
• 3000-3400cm - • caused by (hydroQen -bonded) 0 -H ln a tcol'lol s to asSian a def'in1te
• 2B00- .3200c m - ' duo to ( h yd t·ogcn - b ond cd) o - Jool I n carb oxylic u.ctd s w a v enu m ber.

U nrt 3 and 6: Chemi stry Labor"atory S ki lls 37

 Content Guidance

The peak due t o O H is
not .spli t. n or" doe:. i t.. eau :se
s,plrtt•na.
NMR spectra
You will be .allowed to use tho Edexcel data booklet du ring the assessment.
The POints tO lOOk (Or" ar·e:
• The nurnbcr of peaKs - thls g i ves the nun,ber o f dlff e t·cnt envlrontncnts o f the
h yd r ogen atoms. For e x .amplc. propa n - 2 - ol, CH~C II (O II )C J b, will have three peaks
becat.ase the h ydrog:en atotns fn both CH3 "roups are fn the sa m e environme n t .
Propan-1-01. CH.,C H ~CH~OH, will have four peaks.
• The splltUng pattern - If a peak I s not split, eith er t h o grou p has no hydrogen a t e rns
on adjacent cat'bo n atoms (as In propanon e) o r it is an 0 - H QI'"Ol.I P:
tr tt ts split Int o 2 there Is one hydrog:en a t om on the adjacent carbon atom
- l f tl l.:s split Into 3 then thea·e ttre two hydrogen atoms o n adjacent c-arbon ntoan:s
- I f lt Is split i nto 4 the n the r e are three hydrogen atoms on adjacent C:irbon a t on, s
• The chemical shtrc., 8ppm (see the Ede.xcel data booklet for 6va l ues .):
the t-1 of t he o -H In a l cohols has a cJbetween 2 and 4 pp1n
the 1•1 of the 0 - 1•1 I n ca rbo xylic nclds between I I nnd 12 pp tn
the f.l In Cf.l~ . C f.l 2 o r C l-i between 0 .5 and 3 .5 ppm

Kn o w l e d ge <.. h ec:.lc. 27
Comj:)Ounds A and B both have moleeu les eontain in2 3 ea.-bon atoms and I oxyaen atom.
Assu me t.hat. A is pi"''panone and thal B is pi"'pan-2-ol. Wr"i t.e down t:he observat.ions tha~l
would ba n-~.:~. d o in "tho foll~i na tests.

• (a) Some 2 ,4..dinit..-cphany(hydr.:tZinc was nddod to o::.ch. W r i t.c down you r ob~o,.....,.ati ons
wi'th A and w i t h B.
(b) Some phosphorus(V) chloride was added to each. Writ.e down your obse..-vations
w i th A and w ith B.
(2)

(2)
(c) Eaeh was warmed wit.h acidified potassium d ichromate(Vi) solut.ion. Wr"ite down
you r obso,.....,~io ns w i t h A ~nd with B. (2)
(d) 1-tow n-1.any poaks would thoi'"'O bo in tho NMR 5poc-trum of compound A, n nd
how would they be split.? (2)

Knowl edR<E! c:h ec:k 28

The •nolecules of compounds P and Q contai n 4 carbon atoms. and molecules of compound
R con·t .ain 3 co:u-bon atoms.
A.ssu rne: t h at P is butan-2 -ol, Q is but~none: :tnd thnt. R is propanoic acid. Wri te d~n 1.he
observa-tions Wlnd dGtduc:tions: "th at would bet rnado i n t h o fo iiCJI'I,Nina to5ts.
(a) A ~trna ll p iece of ~todiun-1 was addec:l 'tO Pin an ovapora:tina basin. Writ·o down your
observat-ions. (2)
(b) P was warmed with acidified potassiurr~ dichron-~a'te(VI) solution. Write down your
observat:ions. ( I)
(c) P WD-S wArmed acntly w i t h "" m i xtu re o f iodine ~nd sodium hydroxide solu t ion. Wnte
down your observaotion$. ( I)
(d) l.J5ct your an~twars"tO (a). (b). (<:)and the info.-.-nation i n tha stan-~ ofth a quastion to
identify compound P bywri t ina i t.s nan-~e or formula. ( I)
(e) The infrared spectru m of Q is shown belov.t.

38 Ede><:Cel AS/A2 ChEHY'Iistry

 Unit 6

r so

0 ~~~~~~-r~~~~~~~~~~--~~~~~~--~~~~~~~-
4 000 ISOO 1000
wavenu mber/em - •

What does this indicate about the natul'e of eompou •-.d Q? (2)
(f) Q was warmed w it h some acidified pO'tassium dichr'Omate(vl) solution. Wri't:e
dow n your ob~c.-v~"ti ons. (I)
(&) Use yo ur unswe1-s "to (c),{f) a.nd the inforrTU•tion in the stem of 'the ques-tion -to identify
compound Q. (I)
(h) Som e R. was added "to aqueous sodium <:.arbonate a nd -the a as tested with limewater:

• (i)
Write down your observations.
2cm:. of P and 2crn3 of R were mixed and 4 drops of concentrated sulfuric acid vvere
c:lr-cfull y .:added . The rni >rt.uro W;tS wa.r..,.,od in :. bc;1kc r of hot Wi:l-tor fo r 5 m inutes .
(2)
..
The mixture was then poured into a beaker cont.ain in.a aqueous sodivm carbon ate
and cau"tio u s ly smelled. Wri"te down you r observations. (I)
G) Name the type of oraanic compound formed by the reaction of compound P with
compound R. (I)
( k) Usc you.- ~nswc 1--s 'to {h), ( i) ;:)nd t ho i nfcwrnn'tio n in 1:ho sto~ o f-th o qu os~i on t o
identify t:Ompound R.. (I)

In o r gani c s ub s t a n ces
M Os t o r the marKs are f or observations. v o u wll1 nonnally be expecte<J t o tdenufy
each unknown. and you may ;::l)So b e r e quired to write an equation - e.g. for a ligand
exch anQe r eaction. a redox reaction or for a prectpltatfon reac tion .
A t ypical mark dl.s trlbutlo n t.s:

Obser-vations 9 or 10 rnar"ks
l dcnt:lrfcat:.lon o,. each unknown 2 or 3 '"a.rks
Equation and/or comment I O l" 2 '"arks

V0\.1 wtll be Qtven two or three <1-bl ock. compou n ds as solids o r as their sol utions.

Cations
The c utlons will be limited to cr3 ... Mn, ~. Fe<h, Fc-3•, co-2 ~. Nl 2 ~. cu 2 ~ und Zn2 •; and
possibly K•·. Na • and Nf-1 4 +.
U nrt 3 and 6: Chemistry Labor"atory S kills 39
 Content Guidance

Anions
The an ions wl11 be limited to so4 ot-, Cl- , Br-, 1- , NO;,- and co;:)::t-; plus cro 4 :a:-, cr2 o,.a-
a n d Mn04 - .

Possi ble tests

Appearance of solid
You may be asked to comment on lhe col our ana whether the solfd ts crystalline or
a powder.

Col our Pos s ible Ions

Colourloss Zn2 •
GrCIIon F o-2-, c..-3•, N12 • , Cul:•
Bh.IO Cu:l•
Pfnk Co2• , Mn2 •
O r-Ango C r:~.072-
Yallow c r o .. 2 -
Purple MnO,. -
Appearance of dilute solution
Colour P o ssi ble i on s

• Colourless
G,-.een
B lue
Pink
Zn2•, Mn2•
Fe2 •
Cu2 •
co:t•
, Cro3•. N t2 •

oranae Cr20,.:2-
Yellow cro .. :a-
Purple Mno4 -

Test for a sulfate

A few drops of dilute h ydroch loric acid are added to t h e unknown solution followed
£-::x.-. nll•n a r c-ip by a few drops ofbartum c h l oride solution .
The ionic equation for 'the
Obse .-vadon$ I nference$
predpitatio•'l o f badu m
s ulfato is.: I t IS a sul fat.e

B:al·"(~q) + S0 42-(aq) l> •Son-1crt.irnos th o b;::triur-n chlo..-ido i s .:toddad first., foiiO'Io'Vad by t.h a hydr-ochlo•·i c: ac:id. Tha
BaSO.(s) observations t.h en are whlt.e pr-eclpitat.e ..,... which st.ays on addft..ion of hydrochlor-Ic acid v:'

Test for a halide

/'\few drops ofd tlute n llrlc acid arc added to the unknown soluuo n, ro l lowed by D. rew
drops of s ilve r n itr ate solutlo n .
The solu bility or the pcecLpllate rotmed js tllen test ed tn dflu[e and con centrated
ammonla.

Ede><:Cel AS/ A2 ChEHY'Ii stry

 Unit 6

Test Observations Inferences

Add dllut:e nlt:rlc a c i d <o a
solution of tho unknown
• VVhlt:e prectplcat:e .,;' t:urntna • It:. I $ a chloride
purple on standi ng -"': soluble In
and chen sliver nlt.rat.e• dllut:e ammonia -"'
T ost .:ho proc l plt.a~:
fi rst: wlt:h d ll uc.e ammonia
• Cronn"' procl pltr..to V lnaolublo In • I t Is a bron"'ldo Ex.. m•ner t:i p
The i on ic equat i on for t.he
dllut.e but solubl e In coneentrat.:ed
and t:hen (If n o change) Qn"'monla V p rocipi 'tl1:ti on o f n s i l ver
w i th con ccntrat:cd
ammonia
• Yellow precipitate -"' Insolubl e In • I t Is an Iodide halide (where X stands for
co n con t r ~t:ctd 9 fnn"' Onla .,;' C l, B r or I) is:
•sometJme.s 'the s ilver n it r ate l s added ri i"'S t., fo llo wed by 'th e n l t.t"lc: a c:ld . The o bserv:atJons ror" a Ail • (ac:a) ...,. X"" (ac:t) ~
c h l o ri d e 'lho n - ro whito proci pit;.t o .,;' wt1i c h s t ays o n add it ion o f nit ric ;;ac id ...-: AaX(o)

Tests (or a carbonate

T etst Obso rvation s l n fo r o n cets
t-feat tho s:olld t:est: A gas: Is produced which t:urn c ll""'ow.,.t:or I t Is a c.;lr bonaut
any gas evolved With c.loudy .,;'
llmeweter
Acid+ solid .....
;.,.ny gas evolved w l c.h
Bubbles .,;' (or fl~~l ng or off•rvos:conce)
U mewate ,. t:urns milky/cloudy V
I t: Is a carbona~

limewater

Test (or a nitrate

•
Tes:t:
Add Oevarda's alloy (or aluminium
powder) and dtluto codh..un
Observations

• .,
Bubbles (effervesc ence)
Inferences:
..
hydroxide and w a r m - cest t'U'IY
p c ovolvod: old.,or with a glace rod
dipped 1n concent.ra~d hydrochlori c • White smoke V • I t tc a n i trate
ac:td: or wi th damp red llt:mus • Ut:mus aoe• blue -"'

Addition of sodium hydroxide until in excess

I on Obse rvac:lons after a llc:cl e NaOH added Observa't:l ons aft:er excess Exam•ner t::i p
F e , ... Describe tho c o l o u •- o f t h o
Crean procl plca't:e V which gooc brown o n Proctpltaco s:uays -"'
p rctei p ita"tc;t and whethctr or
cr>•
st.andana -"'
Green preel pH:.at:e -"' Forms g,.een solution ., not i t. d issolv es in excess
:.odiu m hydr o xide.
Nl 2 "" Green precl plcat:.e -"' Prec:Jplc:at:e scays -"'
Cu2 • Slue prec:lpl t:at.:e -"' Prec:lplt:.at:e scays -"'
M n,... K n nwl .,.d g., c h nck 2 9
Off-wh t ~ (buff or sandy) .,;' prec ipitate which Prectpttace c~a.Ys V
da.rken.s on standing .,;' Wr+t.e ~het i o n i c: aqv a:tion s
co>· for addinQ a small amou nt
Blue precipi tate .,;' wh tch goes p ink on P,.ectptU.t:e st.a.ys -"'
st:andlna V o r aqu eou s 50-diurn
Zn2.• Whtc:e proclpttac:e -"' Forms col our ·l aas: sol ution ., 1-!ydn:»<ide «> [C r(H 2 0)6 J>+
ion s followed by excess.

U n rt 3 and 6: Chemistry Labor"atory S ki lls 41

 Content Guidance

Addition of ammonia until In e x cess

I on O b s e t"vac:•ons a r c:er a llt:c:l e NH :~ ad d e d Observat:lon$ arcer excess
Fe2.-+ Green precl plt:ace V which aoes brown on P reclpl cat:e scays V
stan din g V
c.-'- G J"con procl plta.to V P roc l p lt.:lto slowl y dlss.olvos In
eoneentrat:ed aml'nonla co f orm
areon sol ution V
N l2+ C r oon procl p ltaco V Forrna bluo sol u t:l o n V
Cu2• P a lo bluo p•·oclpltato V Forrns dar k b l u o col u t lon V
VVnt.e the 'oni ~ equ;;a.tJons Mn2 • C>f f .. whlto ( buf-f or sa.nd y) V proclplta.t o w hich PJ"ocl p l ta.to 11ta.ys V
for add i 1"1~ a small amount da.rkens on n.andlna V
of o:tqueou :J t~.rnn"ICin i a. Co2.• Blue preclplcace .,.... which goes pink on scandl ng: V S l owl y forms: brown solut:Jon V
to [Cu(H2 0)t,]2...- fans. Zn2.•
followed by exeess. W h lt:o proc:l p l cace .,..... Forma colou rl oas aoluclon .,;

Ugand exchange with hydrochl oric acid

Hydrated copper(u) and cobalt (u) tons undergo ltQand exchange when a few drops o f
c.oncenl rutod hydrochlot· rc o:actd a t·o added.

I on O b servati ons
[ Cu(t-12 o).:r :t• Solut:.l on aoo11 grocn V
(Co( ~.,_O) oJ -1• Solu t:;l on goe s blu e V

• The e quatio n for the r eact i o n o f h ydrated copper(n) Io n s ts:

[ C u(H 2 0) 6 _1 2 •(aQ) -+- 4 C J- (aq) ~ [ C u CJ.,JZ- (aQ) +- 6t-1 2 0(l)

Redox tests
Addrtion of potassium iodide
Aqueou s potassium Iod i de 1s added l oa solution conlalnlng the u nknown tons , which
oxidise the Iodide Ions to i odi ne. Starch solution Is t h en added,

,...-
Io n

Cu2 •
Ob ~ -e r vat:lo n s

R od- b r-own .soluti o n .,;

R od- b row n colou r- V (wtth
S~a r e-h added
B luo- blnck col our V
B luo- blnck col our V
Re<;en:l t h e col our .;afto•- preclpl t.ace)
add • n~ potassium iod1de
c~o,.2.- or cro_.2. .. 1n aeld B row n col our .,.... B lue- black col our .,....
.snd a f t.er' uddi na ::Jt...arel"'.
Addotion of aqueous chlorine (chlorine water)
T hiS IS a redox ceac tton tn whiCh chlorine ox1c11 ses the unknow n lon.
I O I't Obse r-vat:: t on s
Br- R ed colour V
,- R o d - b r own col utl o n .,;;
goe s blue -bla ck V when st:arc:h a d ded
Fe2. ... Goe.s s llahcl y brown V :
t:ho Fe-'• Io n s c;;;an t:h o n be t:es~d usi n g NaOH (Aq )

42 Ede><:Cel AS/ A2 ChEHY'Ii stry

 Unit 6

The I on ic half.. eq u at lo n for the reduction of c hlo rine ts:

Cl2(aQ) + 2e- ~ 2CJ-(aQ)

Addition of other oxidisine agents

l o n t o whlc;h an
o xidis ing ag en ~~: I s
adde d
C ~ .- In alka.llne
s o l ut:lon
Fo2- In ncld solution
O b~o rva tl o n s wit h hydrogo n Ob•orvilld Q n s with l a ad(•v)
pero xide a s ~h e o xidi s ing o xide as ~ h e o x i di s ing agen~
a ge n t f'ollo w ed b y fil t rati o n
Yellow coluc.aon . , (of C rO,. ZJ Yellow coluclon .,., (of C ro,.2 -)
Goes slightly brown . ,; Goes slightly brown .,.,;
t.he Fe~· Ions c-an chen be t.ested che Fe3 ... Ions can chen be
using NaC>t-l(aq) tes t od using NnC> I-I (aq)

Assume that. you have been 2 iven :some solid nyd.-ated c:oppef"(ll) n i t.ra•t e.
Write down -the ob:serv~bons that you would expect. ·t o ma.k.e. The answers a~ on p. 72.
(a) N ote the appear"'anc:e o "ftto\e solid. ( I)
(b) Heat: a small sample o f the solid. Wr-i te down you ,. obset"Vations. (3)
(c:) Dissolve some o f t:he solid in water- and then add aqueou s ammonia. w ith sl'\akinsz.
un-til in excess. V\lritc down your obsorva~i ons. (2)
(d) Dis:sotvc tho rcrn;,indo•· of the solid in w~-tcr ~ nd add pot::l.s:$iu.,., iodid e solution.

• Then add 5 drops of starch sol u~ion . W rit.e dovvn your observations.
(e) W rite an ionic equation . with state symbols. for the r eact:ion 1:h at 1:ook place when
potassiul"r"'' iodide was adde:d::;.·- - - - - - - - - - - - - - - - - -
(2)

( I)

Knowl cod gc c h eck :J2

Assurno tha1: you havo boon a ivon sol"t"'K'K s;olid iron(IO sul fato.
V\lrito down tho obsorv~tions th=at you would GXpo~ t o m.:ak.o. Tho ~nswors :aro o n p. 73 .
(a) N ote~ tho colour of 'tho solid. ( I)
( b ) Dissotvo the solid in wator i n~ boiline tube. T o one po.-tion, add .::.queou s sodium
hydroxide a n d a iiO'IN to stand for a (e'IN minutes. Write down your observations. (2)
(c:) To another portion. add d ilu1:e hydrochloric acid (oiiQ'I.IVed by bariu.,., c hloride solution.
'Wr"i1.e down you ,. observations. ( I)
(d) T o a 'thir-d pol""tion. add some solid lead(IV) oxide and some dilu'te s u lfu.-ic aeid. Warm
acn-tly for 3 m i nutes nnd filter: Tc~t t h o filtr::.tc wrth ~q u eous sodium h yck oxidc.. 'Write
do-.,.....n your observa-tions. ( I)

Knowl €-d ge c. h ec:k 33

Assun""'e that you have been aiven a solu1:ion of zinc bromide.
Write d Q'I.IVn 1:he observations that you would expect to rnake. The answers are o n p. 73.
(a) N ote the appearance o"f·the solution. ( I)
( b) To one portion, add aQueous sodium hydn::»<ide until in excess. W r it.e down your
o~ervation:s. (2)

Unit 3 and 6 : Chernist.ry LabOratory Skills ...

 Content Guidance

(c) T o .::lnc:rthc.- portion , .:1-d d Aquco1..1s arT·u-noni::. unt il in c:~oCCc.ss . Write d own your
observations. (2)
(d) To d -t.h ird portion, add dilvu. nit r-ic: acid followed by aqveovs s i tvar n itTa~.
Write down your obser"Vations. ( I)
(e) To a fourth po1-tion. add aqueous chlorine. VVrit:e down you r observations. ( I)

You must rQcord: • USQ spQc::tr;i~, info rm;ation in t h Q quQstion a nd

the colo u r" before and after the test your obsef"'Vatlons to work oLit t:he Id entity or an
the colo u r of' a ny precipitate unknown
You must. know t h e tests for:
whether or not a preclpttat.e dissolves In excess
sodium hydroxide o r excess ammonia
• aJdQhydes. ketones. carboxylic adds. a lcohols and
alkGtnos
You must bQ ;a biG to:
• wr1te ror ligand exChanQe. Mdox and

Activity C: Quant:it:a.t:ive measurement:

Full details or a ll the exp ertme1ns assessing thiS acuvl ly will be gtven t:o you just:
b e f o r e s t i uUns tho n.sscssrncnt. It Is csscnt.l al lhnt you read them ca r e fully b e fo r e
s t a rting any pr.:.ctlca l work.

You m u sl stop wl•·u~:n
ono d..-op of pot.assi1.1rn
rnanaana~e(Vu) t:ums the
solution p~ l o p ink.
Redox t:it:rat:ions
You will bo required t o tltn:::atc a sol ution of potassium manganato(vu), wh ich Is I n
a burette, with 2s.ocm :) of a sol ution of a reducfng a"ent to whtc h acid h as been
added. NO l ndlcat:or I S needed because t he Ut rauon IS s t opped whe1\ you see the
nrs t pc t· n,a ncnt pink col o ur. This I s due to n s light oxcc.ss of tho I ntensely coloured
Mno.q- I o n s.
The reducing aQent will be supplied as a solid and lt must be welfthed and made u p
t o 2SOcn'l;, In u v o l umetric nask.

You must record aJI
voluM~ t.o 0.05 ern:i. Thu s
a '-"'CC I Un"''Cl .-ocordoc:l ::as
23.6cm3 would lose a mark
- i t s.l-lould be recor"ded
as 23.6-0cn-~ 3 .
P ossi b le erro r s
• Not r ecordtns;r a ll m asses to 2 dec imal p l aces.
• Not rtnslnQ: a ll ll'le reduclnQ agent solution rrom the beaker Into the volumetric
nusk.
• Not s h aking the volun'letri c n ask suffi c i e n tly.
• Not t'tnst n Q o ut the butette with the potassium •nang:anate(vu) solution and the
pJpette with the reductng agent sotuuon.
• Not n'laklng s ure that the p a rt b e l ow the tap o f the burette Is fill e d b efore doing t h e
first ttt r atton .
• NOt obt afnJnQ: two o r more concordant tllres - th e difference between the t arse~n
and the s mallest tit r es you use to calculate the rncan titre must n o t bo greater than
0 . 2cm .:..

Ede><:Cel AS/ A2 ChEHY'Ii stry

 Unit 6

Ca lc ula clo n s
Knowl c:>d gc c h eck 3 4
You w i ll be g i ven tho equation . The two tnost li kel y r eact ions arc:
Man a:..n:..tc(VII) ions cocidise
• Wfth rron(u) compounds as the l'e<lu c~ ng: aQ:ents Sn:!• ions -to Sn 4 '*" ions ;:and
5Fe2 -"(aq) .... Mno .. - (uq) .,. a t~l -"(aq) - 5Fe""·caq)-+ M n.2"-(aq) .... 4 1-hO(l)
are reduced to Mn2 .,. ions.
What i:s the ratio o f Sn:l•
where the number of moles of Fe2·= 5 x the •notes M no .. - to Mno.. -1
• w ith C lhaned lo lc uctd.- I-12C204, or ll:s salts as t·cduCing agents
6C 2 0 4 2- (aq) + 2M n 0 4 -(aQ) + 1 6H•(aQ)--. I OC02 (g) + 2Mn2 ... (aQ) + 814 2 0(1)

w h ore the nutnbor o f moles ofc 2 o4a-- ~ • t he n"''ol os M no4 -

2
Note that the reaction between ethanedtoate ions and ma n ganate(vu) to ns Is ver-y
s tow at room temperature. so the actdtfled. ethaned toate .sotuuon must be heated
before be1ng titrated.
A typica l mark scheme IS;

Table o~ masses and c tcres 2. m arks

Cal c ulaclon of mean ctcre I mark
A ccuracy or t:lt:raclon 7 mark s
Cal c ulat:lon 2 or 3 ma.r-ks

•
CorTUT'Ioent:s I or 2 ma.l"ks
..
9.51 sz of an iron (n) t:On'\POUn d, Z. wa.s waiszhad out, dis:solvad i n watar 4lnd ""ado up "to
250cm3 . 25.0crY'I 3 portions were pipet'ted i nto a conical flask and sorY'Ie d ilute sul furic acid
added. This solu-tion wa..s then t itrated w i t h 0 .0202 rT'Iol dn'\-l pcrtnssiun'\ n-oa.naan:tta(Vl!}:
Sl=e2+-(a.q) + Mn04 -(.::..q) + a .....• (a.q) _.. SFe.l• (aq) + Mn2•(a.q) + 41-4~(1)
and the •nean t i tre w:..s 2 ....0Sc:n-ol.
(a) Calcu late the mass of Fe2• in 250 c:rnl of solvtion. (3)
(b) Calcu late the pen:en'la,ae of i•"'n in the solid Z . (I)
(e) What would be "the effec-t on t:he mean tit:re and the % of ii"''n if some: of ·the
c;on'\pound Z h ad not beten WO!IIst-.ca.d intt:;. t h a '-"' i umo'tri ~: ft;~~sk7 Justify your •nswar. (2)

I. 59 a of a ar-ovp I etha.nedioattt salt.. M 2 C 2 0 ... was waiahed ou't. di&Solved in water a.nd n'\a.de
u p to 250c:~. 2S.Ocm3 alic::juots vvere acidi fied and heated to 60°C. The I'\O·t solution was
-t:itrntad with 0 .0202IT"tCCI drn-3 potns=:;;iu rn rnnnaan n'to(VII) ~ l ution. T h e .-neon ti-tro w::.s 23.6Scrnl:
SC2 0 4 2-(:tq) + 2 M nO... -(a.q) + tb......r+-(a.q) - > I OC~(a) + 2Mn2•(a.q) + 8._.20(1)
(:a.) CAic:ulntc the number of n-oolcs of crthancdiontc ion s in 250c:n'\3 of t h e sol ution. (3)
(b) Usc your a.nswe•· 'to (a.) to ~ l c: u la:te the molar n·u•:ss o f M 2C:!04 , a.nd h e n ce the identity
o( t h e IZI"''UP I metal M , (2)
[R.elative awmic masse~ L..i = ~.9: Na = 23.0: K = 39. 1. Rb = 85.5]
(Q StatQ a n d explain the effac't on tho fit"S't. titre if the bu •~ette ha.d been wa't w i t h water.
and not. rinsed out with some potaSsium rT'Ianaanat.e(VIt) solution. (I)

U nrt 3 and 6: Chemistry Labor"atory Skills


sur e t h a-t you record
.sll .....olu n'\es to 0 .0 5 C.I'T"'J
a n d a ll pH valu e s to I o r 2
'--'\e<:onoal places.
Content Guidance
pH t:it:rat:ions
You will be ask e d t o rn easure out. using: a pipet t e, 2S . Oc m~ of a solution of a weak
acid and measu r'e tts P H u sing a P t'Obe and pH meter'.
A s tro ng alkali , s u c h a s sodium hydro x i d e, of kno wn concen tration I s the n add e d ,
Initia lly 1n s n1a 11 a m ou nts of between 1 a nd 2 c m 3 to Qet a r ouQh idea oft h e equ ivalen ce
potnt. Thl.s IS t hen repeated but addi ng the a l kalt In larQ:er' amount s un\11 c lose to
tho cqulvulcnco p o int. when lt I s then o:tdded In o.s o r I .Ocm .:t portio n s. Anor each
addition , the p f.l o f the soluti o n t s m easured . T h e a dditio n i s conti n ued until an e x cess
or a t katt has been ad.d.ed.
You will bo requ i red t o plot a gro.ph o f pN nga l n st volunlo o r ulknll, and then perfo nn
som e calcu l ation s and n1ake comme nts about accuracy.
Error s in t echniqu e
• As with all utrauons. make s u re tha t you rtn.se o u t the pipet t e a n d bur'ette wtth the
appro priate solullo n s .
• Make su r e t h a t the part o f the bu r ette below the tap rs fill ed bef o r e s tarting the pH
titration .
• Mnkc s u re t hat you add the a l ka ll In s n 1u ll .un'lounls to s t c:l l"t with and close t o the
e n d pornt. I n betwee n these it ca n be added in 5 o r l Ocm.;) portio n s .
• Make su r e that you sur t h e solution thoro1.aQ hly with t h e pH probe after each
ad.dltton o f alkali. Fatlure t o do thfs proper'ly ts a common error.
Graph p lotti n g
• Make s ure that y ou u se at l east h alf the g r aph pape r - d o n o t draw a tiny g r aph a t
t h e bottotn left of the g: t·aph paper.
• Make s ure tha t you label they-axts <P H ) and the x-axts (volume of alkal1/em 3 ) .
• The p i t value before any a l ka li I s added s h ou l d b e about pit - 3. It should n so
s h a r p ly over the n ext 2 to .3c m ~ <il nd the n nat ten o ff. slowl y rnc r east n g befor e ri s ing:
ahnost venrcally as the equ i va lence point IS reaChed (when the acid and the a lka lt
a re In a 1 : 1 ratio by m o l es). ll then nntte n s o ff again artcr abou t scm.:t o r e x cess
a lkali has b een :adde d .
To see what t h is l ooks like. look at the g: r aph or the a n swer to Knowleelg:e check .37
on page 73.
The buffer r eg fon runs fro m a fter th e Initia l rise I n pJ.I (after about Sc m ~ ::.lkall h ns
been added) to about scm ;) befor e t h e a l m ost vertica l pan. Thts fs when t h e r atio
or [weak acldl: ISa l t J varies rrom about~: 1 t o 1 :0.
A typica l n1ark sch e n1e I s :
T abl o o~ r o a dingc ""' or S m a r ks:
Gra ph 2 or 3 m a r ks
A ccu r ac y 2 or 3 m a r ks
Cal c u l a'tio n c- f"ro ,...... g r a ph 3 ITI'<lr ks
Corn rn e n c.c- I or 2. mar ks
Ede><:Cel AS/ A2 ChEHY'Iistry
 Unit 6

K nowl cdgC'l c h cc. l< 37

25.0cr-nl of a solu 't:i on of a weak Acid ._.X was ~cnsu.-cd i n'to o beaker a.nd its pP-4 I"T"tel:l.Sur-cd. A
bu•-.atte was filled with 0. 1 2S ~T~ oldrn-l sodiurT'I hydn:»<ide soh.rtion . T his was added a l ftt;IQ at a
time. with stir"l""injZ, measur"ina the pH after eac:h addit ion. The ~su i ts ar"e shown below.

V o luf'ne o r a.lka.ll/cn -.2 pH V o l urn ~ o r a lkali /c.,.,~ pH

0 2.9 19.00 5.7
1.00 3.8 19.50 5.9
8.8
2.. 55
s .os
1.3
1.6
20. 00
21.05 ......
7 . 50 1 .7 23.00 11.7
1'2. SO s .o 25. 00 12.0
IS.OS 5 .2 30. 05 12. 3
17 , 5 0 s .s 4 0 . 00 12 , 7

(a) Plot a 1Va.Ph of pH o n -t.h e y-axi5 a.aainsot '-'Qh,. lrrua of sodiun"' hyclroxide o n the x-axis. (~)
(b) Use your araph to find t:he voh.Jrne o f a l t.Qii needed to reac:t with t h e 2S.Oc:m l o -f t h e
acid. HX (3) and the pH a"t the equivalence point ( 1).
(c) Use your answer to (b) and the concen'tration of the sodium hydroxide solution aiven
to cnlcuiAtc the con ccn 'trution o f the ucid. I-IX. (2)
(d) MeASUI""C the p~ ~t the point. w hen h o~d r the acid h ~ been neut.rA-Iised, And hence
calc:ulato t ho value of pi<.,. Q f tho ac:id I--IX. (2)

• (et) Usa you r ;ansvvc. •~ to (d) to c;alculortet 'tho v""luo o r K.. of tho acid .
(f) Ovo•-wh .=at p l-1 r;r, n ao would t ho solutio n in the. pl-l tl't,ra:tion bet able to act =as .=a buffetri
(I)
(I)
..
(a) Cornrnc.nt o n tho .:lC:C:Urucy of 'this !T"'c:rt.hod few fin dina the. CC:WICOn'tr.:atio n o r thet Acid
compared w ith a normal acid/base titra1:ion. ( I)

Exa.nt iner tip

Kin e t:ic e xpe rim e nts You IT"' U ! i t n::aad tho
in stn.Jct.ions completely
Following a reaction at con stant temperature befor*e star-ti na the
gxpor in'\Gnt boc;ii\v~o . onc o
T h is t ype of expertment ts perfot"mecl to ftnd t h e Or'der or reaction or one of the
you h ave started, there wi If
t•euct ant :s.
not b e time to work o u1..
Full details will be Qtven and ca r e m-...st be taken t o follow these Instructions ca r efu lly. w h <tt to do n QXt.
The procedure waH be:
( I ) Measure out the rcngcnts nnd catalyst solution s fn two sopurntc beakers .
(2) Prepa r e t h e quenching r eagent in a con ical nask.
(3) Flll a bur'ette with a sol utton that wl ll r"eact rapidly with one rea"-ent (Of Pr'Oduct).
(4) Mix tho content s of t h e two beakers a nd st<l rt n c loc k.
(&) After 5 minutes r en'love a I Ocm,:, s:.n'lple. quen c h t h e reacuo n a n d titrate against
t h e solution tn the burette.
(6) Remove f u rther sampl es every 5 minu tes and quench and tnrate.

U nrt 3 and 6: Chemistry Labor"atory Skills 47

 Content Guidance

Kne>wl c dgc c:_h cc.lc. 30
Why rnu:s.-t the
<:on <:Qn l.ration r; of
p..-op.ai"\\ne and ac:id be
much I~ •"'Wcr th~n t h .:.t of
the iod1ne solution?
This n'let.hod can b e u sed to find the order o f the r eactron between propanone and
Iodine in the p r esence or an acid cata lyst :
Cl-t~COCH,:,(I) -T 12 (aq) H- cat a lyst 0) CH~COCH 2 1(aq) + H1(3Ct)
The iodine t n t h e sa mples removed is tttrated against sodium th iost.alfate solution .
A t ypica l n'lurk :schcn'le IS:

Tab l e o r volumes o r reagenc: s , c:l c:r es and t:lrnes 3 0 1• 4 marks

P l o cc:l n g o r graph 2 0 1· 3 marks
l nt::c rprc C:at:lon o r grap h 2 o 1· 3 rn~r ks
A cc urac y o f exper im e nt:: 2 m arks
Co""'""'c nt:c on ex p erime n t: 3 o 1· ,._ rnnrk.s

K n owl ~ dg e c h ecl < 39

Usi'1a a t'T'Iea;urinsz c:ylin der. 25 c;.,.....l of a 5elution of propanon e wa& m ixed with 25 c:m 3 of
d ilu te sulf udc: acid i n a beaker. 2Scm:. of a dilute iodine solu"tion was 1neasur.ed o u t in another
rno:..sur-inw cylinder.
U sina a. thir·d rnc~~uri na cylinder, 20c.m3 portion!S of sodium hydroacnc.arbon~tc solution wc.-c
put into c:onic:al flasks.
A bur atte was filled with 0.0500 mol d rn -3 sod i un-~ -thio;:ul fate solution ,
T h e iodine solut ion w~s poured in-to the beaker- c:-on tain ina the propanon e and ac:-id, stil"rec::

• and a dock started. After 5 m i nutes, IOc:.m:. of the reaction mixture was rernoyed and r"un
into the sod ium hydroac n c.;:u·bon:lto -to quench tho rc.:~.cti on. Thi :~ w:...s -th en irnmcdiotoly
tit~d ~th t h e sodiu""' thiosul fate solution .
Another I 0 c.~ portion was "th e n removed. quenched and titrated. until five portions 1-\a.d
been r-emo.....ed. The r-esutts af"e sho.......n belovv.

Vol u t'ne o f V o l ur'ne o r V olu m e of V olu me o r s o dium

pr-opan one so l ut:ion / sulfur ic acid / Iodi n e sol u c ·ion/ hydroae n carbon ace
em> e m > c n -,.3 solu t:lon /c""'3
2S 2S 2S 20

T fm e / ml n IS I 10 I IS 20 2S I
T lcre / c n 'l , I 18 .0 I 14.4 I 10 .8 "7.6 4 .0 I
(a) Plot a i!'raph of t itre on t h e y-axis aaainst time on the x - axis. (6)
(b) Calc:ula'te the s lope (~radien't) of this araph. ( I)
(c) VVha't does the slope of t h e i;Zraph measur e? ( I)
(d) Use you r answer 'to (c) to find t he order of the reaction ""''th respec:t to iodine.
J ustify you ,.. a n s-"C:~ (3)
(e) In this experi ment., -the concent.ra'tion of propanone was rn ud"' l ar-Eer than that.
of tho iodin e . Why isc this n oc:ossa•-,.1' ( I)
(f) \Aihy is i t not n ecessary to use a pipcrtte 'tO rno;u;ure tho volu m e of propanone.
sul furic: acid and iodine soll.ltions? ( I)
(a) Why is i"t necessary to add the reaction mix-tur e t.o aqueous sodiu""'
1-.ydroaenc:a,.bonate? (3)

Ede><:Cel AS/ A2 ChEHY'Iistry

 Unit 6

( h) Wha.t would bo produced jf ~d i u rn h ydroxid e ~ nd not :sod ium hyd roa cnc:u- b onat.c
h ad been used~ quen c h "the reac:tion ? (I)
(i) t-low wovld you m odi fy t h e proCQdut'"Q ~ e n able t.he o r der wrth re~pec:'t ~
p.-opanone be found? (2)

F i ndin g c he acci vat ion e n e r· g y o f a reacci o n

T h ts metl, od requtres t he tlme. c. ror a patu c u lar stage tn the reactton to be •neasu1·ed
n t u certa i n t c 1npc r atu rc, T. Tho oxp o t·l n ,cn t Is t h on repea t ed at d i f f e r ent tempe r atu res.
T h e A rrhe n ius equation connects t he activation e n e r gy to the r a r e con s t a n t of t h e
•·eactlon:
IOSaok - ~ x - 1-
2.3R T

where R ts the gas constant and T as the t empera t ur"e tn kel vin.
-~
A g r a ph of log 10 k ugul n .st TI wl1 1 s1vo a straigh t line o f slop o 2':3R'·
H owever. t he r ate constant I s dttTIC\.tlt to measu r e and a g-raph or
lot;r(ra t e), o r the
t og o r anyth ing: pt"oporuona l to t he ra t e such as 1/C, wtll a l so g i ve a stratght l tne
o f slope - €.., .
2.3R I I - C,.
, - IS plotted aQal n st -::;=-• the S l ope IS
I ( a Qrap h Of IOR1o - . ~R ,
2
(See t h e unsw c t· t o K n owledge c h eck 40 o n page 74.)

• A typtc.a l m a r k schem e i S;
..
Table o f r e a din gs + cal cula.~fon o f l og + a n d ..:- S or 6 ma.rks
Plot:t:"lng graph a n d lnc:erpret:acl o n 3 o r 4 markS
C aJ c:ul a cJo n a nd a ccurac y o r a cclvac.l o n e n e r g y 4 marks
Cornrn e ncs I or 2 marks

A ctivation energy or the reaction between sodium tlllosulrate and acid

Sodium t.htosulfate r eacts w i th n itr ic acid to produce a precipitate of su l fur:

S:;z0;,2 - (aCJ) + 2 H • ( aQ) ~ S(S) + S02(aQ)-+ H :z0(1)

T h e experime n t I s des ig n e d to tf m e h ow lon g I t t a k es for e n ough sul f u r to be p r oduced

t o htde a cross on t he reacuon vessel when looked at t hroug:h the reaction mtxl ur"e.
The expertment t.s r epeated a t different te 1nperatures.
K nowl edge c;.h ec;. k 40
A C:t"OSS was 1"1"\&r'ked on the o u tside of a boilina 'lu be w i th a b lack w~ter"pr-oo r marker. 10 em:3
o f a solution of s,odiu rn 'thiosvtfat.ct was pvt in t h et boili n ,a tube a n d its u.n-.pcu-..t u r ct measur ed.
I Oc:m, of dil ut:e n i t.r k acid was put in a t.es't 'tu be. This was t:h en p oured i nt.o the boil ina t.ub e
and the solu tion stin-ed w i th a ther"TT"Iorne1.er: Tke t irne taken ror" the cross t.o become invis ib le
was r ecorded a n d t.he t.ernpera'Wna of 'th e solut.ion rcrt:aken.
M ona sodium thiosulfa.to a-nd n itr ic: a.c:id wore 'then wal"n"'etd separ atety in a beaker o f watcu- a n d
the experiment repeat ed.

U nrt 3 and 6: Chemistry Labor"atory S ki lls

 Content Guidance

The 1-osults .,,-o s h own below.

TJm o. ~ /c I nitial t o mpo r a turo/°C Final M o an t o rnp c ratu r o / o c

c:ern p e r-ac u r-e/°C
120 20 22 21
5 .. 35 35 35
26 so ..a ..9
IS 62 58 60

- 1- ls- • lo a, o- ,I - M e a n t-e rnp e ra.t:u re. TI K ~K-•

•
0 . 00833 2.08 294
r
0 .0034 0
0 .0 185 - 1.7 '3 308 0 .00325
0 . 0385 - 1 .12 322 0 . 003 11
0 . 0667 - 1.1 8 333 0.00300
Thq &IOtlPh s h ould h ave
- 1.0 at. the top o f t he (o) P lo t a a..-.:aph of lo,a 10 aa~ins't I (3)
kc,l v in ton"'lpo.-~1:u l-o
'tirno
y--axi:J a o ina down 'to - 2 .2
(b) What does the shape of t he aro.ph tall )"QU abot.tt t h e relation s h ip be'tWaan t h e r ate o f
and 0 .00300 o n -c:h e left react ion and t.h e temperatu re? ( I)
aoinw u p 'lo 0 .003-10 on t h e
ris ht: o n tho X • ::a.xis. (c) Use you r ara.ph 'tO calculate t h e s lope of t:he line you h ave drawn . ( I)
(d) C a lculate the activation e n ersty of the reaction . G ive a s ian a nd units with your ansvv'EH: (3)

• (e) Why d id t h e temperat ure r ise slisrh-dy in the first exPeriment?

Activation energy of the reaction between magnesium and acid

This Is a n o the r experiment thut t.:s ~ ull ab J c f o r n 'lc<:t s url ng the ume t a k e n f o r a ccrtn ln
( I)

point t o b e r each ed a n d for r epeat i n g at differ e n t t e mpe r atures.

I f a larQ:e exc ess or a c id IS u sed, t he tate or reacuon wr ll be approxtmat e ly const ant
b ecause the s urface a r e a o f t h e tnag n csJurn ribbon d oes n ot a lter s i gn i fica ntly. Thus
t he ra t e I s propo r tion al t o 1/ tlme , whe r e t h e t i m e I s t h a t for t h e m ag:n esh.tm ribbon t o
disappear (See Test quesuon 6 on p . 68).

Read and record: • only use con cordant titres (±0. 2c~ when
• a ll m assGts 'to 0 .0 I g calculat ing t hG m a:tn t itrQ
• :..II volurnas in th:r ations t o 0.05 crnl • don't IQaVQ thQ tunn Q I in thQ top ofthQ bunOl'ttQ
• a ll p l-l v.:aluas t o :1t loast one d acirn:tl p l;lc:G • re;~.d t hQ quGst.ion c;;~:no.fu lly bGtf o r a sbrti n g .- kin etic
Oos and don'"ts.: exper iment. to make su re t h at you knOW what to do
e IT\ak.e su re that you stir the solution with the p H
pro b e b GI'for a taking a t·Q;ading
• sh .ai<Gt thGt fl~sk t h orou ghly w h Qn m~ki ng up ;a
solution

Ede><:C e l A S/A 2 ChEHY'Iistry

 Unit 6

Activity D : Preparation
an all preparauon.s. you wall be asked to work out the petcent age yteld. , .hiS will score
3 o f the 12 mnrks I n the assessment.
T h e method Is:
( I ) work out t he molar masses or bOth the reac tant that you measured out and the
product.
(2) use the expr ession nun1ber of moles = mass to Cillcu l ate the number or
moles or reactant. molar mass
(3) I f the roactuntnnd product aro I n a 1 : 1 j'Otto I n the balanced equa tion f or the roilcUon, E xautine t• d
the theoretical number of moles of product - the n umber of m oles of reactant. The pci""Ccnta.ao y ield is not
(4) The theoretical mass or the PI'Oduct = moles x molar n'lass . mass of product x 100.
(S) 96 y teld =ac tual mass of produc t x 10096
rna.s:s of r-eactant.
theoreuca l mass or proauct

Organic preparations
You will be asked to p t·cparc un organic compound and then purify lt. F inally tts
rne l tlng or bo iling point will be n1 easu r ed.
Pull details or the procedure wil l be Qtven and you should rollow t11em catefully.

T e c h nique

• • You must know how t o set up apparatus for s lmplo distillation (see p. 32) and f o 1·
heating under rent.ax, as shown bel ow.
..

Condenser
W::ltef' l n -

Round· bottornod n :uk

E x a ruine r t:i
• Make sure that the water flows into the condenser at the botton1 and out at t h e top. All masses m u st. be
• Check that all the JOints ate rtrm and that they wtll not leak. rec:on:led to 2 dec:uTial
• W h en carrying out dlstlllo:ttlon, c h ock that tho thcrmon1ctor Is opposite the entrance places and volun'les to
of the conden ser . I cml. Mcltina and boilina
• You must know how to recrystalllse a solid. tempera-tures should be
• vou must know now to measure the m.elunQ point or a solid. r-eeol"'ded to I qc.

U nrt 3 and 6: Chemistry Labor"atory Skills

 Content Guidance

M ethods of measuring mel ting temperatures

There arc two con'ln'lon procedures .
( 1 ) Thi s method I S o n ly to be used tfyou: have s ufffc;lent amounts of the sol id . son-.e
or the purlrted solld Is placed In a botltng; or test tube.

-
f-.
.........
H eat
vvt.lter or- 0
Solid under wst:
11

/1 1\
The water or oll IS heated until the sotrd beg: rns to rnett. NOte this temperatul:'e.

• Now r e m o ve the t ube f r o m t he beaker and allow it to cool whfle sttrrrnr.c t h e m o lten
solfd with the thel'mometer. Note the tempecature at whrch soltd nrst begins to
ronn. The melting tcn'lperat urc l:s the mean of thes e two val u es.
(2) Thi s n 'lethod should be u sed when sn'lall an'lounts of solid are available. Take a
capii Ja.-y tube that has been sea led at one end ana nu It to a depth or o .scm with
your purified solid.
Attach It, us i ng a n .•bbe r band, to a thermometer and rnsen the thel'"m o m eter In a
water or an on bath.

T hermotnecer - - - - -H

R u bbo ... band -1::::tf1r~-4_j

-+--OH or watef" bath

~2 Ede><:Cel AS/ A2 ChEHY'Ii stry

 Unit 6

l l eat the bath qu ick ly unti l Its tempera ture r each es about 20°C below the exp ected
m e l ti n g poi n t . Then gradu ally I n crease the temperauu·e u n til the solid melts. N ote
th is approxt1nate •nei UnQ: t enlperature.
Let the o il o r water bath cool s llshtly, and r e p eat w ith another sa mple o f the
solid tn anot h er' capi llary tube. H eat gently u p to close to the app roxtn1ate n"leltlnQ: Make sure that you stir
t e tnperature or t h e soltd, as fOund earH er. Record the t emperature a t whiCh -thorouahly all "the time that
I t I'TlC)ts. you h c~t -the liquid.

M a r k ing
T h e mark. sch eme for organic p r-eparation s wil l be sfmtla J" to the fol lowi n g :

Tabl e o'f ""asses and/or vol un-.es 2. fT'Iark$

Calculation o'f cheoreclcal yield and actual % yiel d 3 fT'Iark.$
% yield > .SOX. fo r 2. markS
~ 1 0% but < SO% f o r I I'T'tark
D oscr ipt:i on o'f product: I mark
Va l ue o'f n-.altln a o r boili n g t:en-.pe,..atu,..es ,.'2. 2 rT~ a rkt:
%50 - I mar'k
Con-.n-.cnt:• 2 m ark$

P repa r ation of aspir i n

Aspirin I s a solid phenolic est e r made by the reaction of 2 - h yd t·oxybenzo lc acid

• (sa l icyl ic acid) and ethanotc an h ydride In the presenc e or p 11osphor1c aciCl ca t a lyst:
..
+ C H ~COOH

Saucyttc acid Asplnn

some 2 · hydro xybon z.olc a cid I s w eigh e d out and put in a dis tillatio n fla sk t ogether
w i th excess ethano rc an h ydride. Then s drops of' phosphoric act d a r-e added and a
tenux condenser &s nued. The tnlxtu re IS heated on a botltng water bath ror 6 minutes
und then some water Is car e fully a dded d ow n t he refl u x condenser . This hydro lyses
the excess e tha noic anhydr-Ide.
T h e mtxt ure IS pou red Int o a beaker or cold water and s t ood tn an tee bath. The Exa m i n or- t:i
Your mass of p urified
rn l xturc I s Oltcrcd u s i ng suctron filtratio n . a nd t h o solid o bta i ned I s rccrystalllsod
aspirin $t\ou ld be
u si n g hot water.
sin""' il;~.r "to tho rna$s of
T h e pure. dry asptrtn ts w e tghed, and nnally t he mel ttnQ temperature o r the aspirin l.s 2-hydroxybenzoic acid
1noasurod. T h is s h o uld be bet ween 13 4 and 135° C . or-ia in a lly taken .

U nrt 3 and 6: Chemistry Labor-atory S ki lls


Wkat i s the ~yi eld if0.95Sil
of aspirin had boon rn:1do
from I.Oa of salicylic acid?
•
Make sure that you use
t.h e m inim u m ..t~o u nt
of h ot crt.hocan o l w h o n
recryst.aJiis•niZ t h e product.
su re that you •· y i e l d
ts at
le:ast O .Sw per I c:m l of
meth yl ben zoate
Content Guidance
The follc:J"o~Vina questi ons ~ •-e nbovt: the prc~a.ti on of nspirin.
(a) De~ribe the app e::u-~nc:e o f your s~.rnpl c of a.sp irin. ( I)
(b) Calculate the -theorertic:aJ y i eld o f aspir in st:artina with ~1. 00a o f 2 -nydi"'X'yben:z.oic: ac:i d . (2)
(c:) Why i s "the a.c:tu.::tl y ield less th.::tn I 00%7 ( I)
(d) Why i s i t: necessary to he.:t"t -the sample s lowl y (at a b o u t. 2°C pe•- m inu te dose to
t h o rnoltina poin1;) w h g n m oasuri t"W' t.hca m olting 'tQrnpor atur-G? ( I)
(ct) Wh~t typo of i mpunty fs r-GI'1""'t''Vod j,,
t h et first fi l t r a1ion durin a roc:rys~ llis;rtio n ? ( I)
(f) What typo of i mpunty fs ral'1""'t''Vod in t:h a soc:.ond fih~t:ion durina roc:ryst:lllis.;:.t:i on? ( I)
(JV Wh:rt would bo fo •-mod if 2 - hydroocybcn zoi c: ac:.i d w;~s wArmed with IT"'Itha n o l in tho
presence of concen t r ated sul furic a cid? ( I)
Preparation of methyl 3 -nitrobenzoate
M eth y l 3-nltrobenzoate Is a solid ester 1nade t>y t h e n ttratton of methYl benzoate.
HNO~
A known volume of m e thyl be n zoa t e is carefully m ixed with so m e con centrated
su l furic acid tn a nask. A nitrating mixture or cooled concentrated sulfuric and nitric
acid t s the n added tn s mall potuons and the temperature maintained between 5 a nd
ts<>c. The fl ask Is allowed to warm up to r oom t e mperature und l eft to s t and for 15
minutes . The con ten ts are then poured o n to some Ice a nd sun·ed . The m ixture Is
filtered u s ing s u c tton. and the solJd was hed. wtth a llule tee-col d ethanol.
The solid Is the n recrystaJiised u si ng eth anol as the sol vent and I s allowed to dry.
When dry. I t I s welghea and Its rne l tlng potnt I s determined fn t h e usual way. 'Th e
metuns. potnt should be between 78 and ao• c.
T he f ollowina questi ons are about the preparati on of IY'Ieth y l 3-nitrobenzoat.e.
(a) Describe the a ppearance ofyour product. ( I)
(b) Calculate the theoretical y ield of methyl 3 -nitrobenzoate startina with 5 .00cm3 of
meti"tyl benzoate (den:si ty = 1.09aci'TI-:l). (3)
(c:) If the mass of you ,.. pr"''du c:1. was 5.05 a . what was you ,.. 96 yield? (2)
(d) Why mu~ t:ne t.empera-ture d u r i na the nitration be kep-t at or below I"'om
tctmpor-;~~tuf"'Q7 ( I)
(o) ldontify t h o oloc:-troph ilc in this 1-o;action . ( I)
(f) Why i s tho rac:ryst:.:~~Ui ~od solid w~shod wrt.l-. a li ttl e i c:o ~c:o l d ot::h .:ln ol bofora bain,e allo""'-'-d
~odryl ( I)
Ede><:Cel A S/A2 ChEHY'Iistry
 Unit 6

Inorganic preparation
You wfl l be given ful l Instruction s which m ust be followed c&r-e fully.
vou will be r equtred l o prepare a soHd contatntng a COJnpl e x transtuon m e tal 1on,
s u c h as ( Cu(NI--1,:,) 4]2 •S0 4 2 - or c hro mlul'n( u ) e thanoate, [Cr:r.(CI-I.;,C00) 4 ( 1-1 2 0)2} .

Pre para t:io n of t:e t:raamm i n ecopp e r(ll) s ulfat:e

C u S0 4 .5 H :~O. Is weighed out and dissolved In the minimum
some solid coppef(n) su l fate,
or watef. Aqueou s ammon i a sotuuon IS added s t eadily. wtth sUtf'lng, untll In excess.
Eth anol I s added to thi s solutio n and a precipi tate of the copper(n) complex sal t
rcu( NH 3 ) 4 1S04 Is formed . T h ts ts separat ed rrom the aqueous l ayer by suction filtration
and the solid w ashed with e tha n o l and allowed t o dry. Finally It ts weighed.

A typica l mark sch e nl.e for .:1n In o rganic p r e paratio n I s :

Tabh;t o ' ma e••• '2 or J n-~;:arks:

Observadon s du r i n g t h e prepara~lon I or 2 n-~arks:
Appearance o f product I or 2 n-~arkc
C:a l c:ula~lo n of % yie ld 3 mar'k$
Value of yield I or 2 marks
C:ornrnenc:s 2 or 3 marks

• E.rrors In t:echnlque
• Di ssolvi n g the solid In too tn.uch water.
..
• J....eavrng behind som e o f t h e solid prod ...i Ct before suction fl l t r a u o n .
• washtng; the l11terea solid. wt t h too 1nuch solvent.

E.rrors In recording
• N o t n 'lnkt ng s ure tho.t al l tnasscs aro recorded t o 2 d ecimal placos - a n ·u1s.s written
as 1 2 . 6 wtll l ose a m a rk.
• Not checktng, a ll subtr"acuons when wotklnQ out the rnass or solid t aken a nd the
mn .s:s o f product.
K nowl edge c.h ec. k 44
The fo llowina c:)uestions assu me ·t hat [C u ( N H3) 4 ]S0 4 has been prepared.
(a) What would you obse........e as t he ammonia solution was added to -tke copper(•)
culf".atct s:olution 7 (2)
(b) Det5Cribo t:h o ;:a ppca::ror.a n ~ o f ycn.u- produc:t. (2)
( c) Assun"'i na'th.:rtyou took 6 .00gof solid hydr.::atod coppor-(10 sulf ::.t:a, CuSO .... SI-J20,
calculate t h e t:heore1:kal yield of 'th e complex salt (Cu(N H~) ..]SO... (2)
(d) Assun"'inathat you made 4 .68 a of product, what. is your y ield? (I)
(e) Nam e t h e type of reac:tion betvv<een hydrated c:oppe..-(11) io n s and exc:ess am ~ni a, (I)
(f) S uaszest a reason w h y t he y ield •s less than 100% . (I)
(a) What was the purpose of addin.a e'th a n ol 'tO -the r eaction m ixture? (I)
(h) \1\/hy was the produc;t wash ed ........tth eth a n ol aft:er suc:tio n fil "t,r ation 7 (I)

U nrt 3 and 6: Chemistry Labor"atory S kills ss

 Conten t Gu i dance

Pre para tio n o f a c hro mium(ll) eth an o ate complex

Weigh some .sod1u1n dlchrotnntc(v•). dissolve tt I n wo:u.c r und pour the solution Into a
round - botto m ed fl ask. Add a n'lfxtu r e of p owdered a n d g r a nulated z inc . P o ur SOI'n e
satutated sod tum ethanoate solution Into a botllns: tube and asse•nble the appatatus
as In the diagram below. carefully add o mixture of concentrated h ydroch loric acid
and water n'lade up In a 2: 1 ratio. Make sure that the scr ew cap ts l oose.

Bolflngtubo

SOdiu m d lchrorn:lte(v.), - --l-- Satu rated sod.l um

hydr-od"'lo rtc: acid eth:anoate
:~ond
-zinc;

The dlc htomate(v•) tons al'e rtr'St teduced t o Q1'een Cf"3 .. tons. and then t o blue ctz.. tons.
When t h e solution Is blue. screw t h e cap s hut. Tho solutio n of c.-2 ... Io n s Is f o r ced out
Into the sod h .am eth anoate solutio n by the p r essu r e of the hydrogen bei n g: produced.
1'\ rea preclplt.al e or the neuLral chrom tum(u) complex JCr2(CH .:,C00> 4 <HaO>:aJ IS formed.

Filter thi s precipitate unde r suctio n . \.Vash it with a trace of Ice- cold propanone and
weig h it .

• Knowl e d ge c:.h ec:.k 45

The follovvin_a Questions are about: the preparation or a c h rorniurn( IO ethanoate complex.
(a) Calculate the 'th eore"tical y ield of the c h romiurn(ll) ethanoate complex - assume
t h a:t y ou took 2 .22a of ~od i u m d ich.-.ornntc(VI) ( 2)
(b) Calculate the 96 yield of 'the exper iment - a~.:surne tha t you rnudc 1.9 1 a of t h e
complex. (I)
(oe:) \1\ft-.y is. t h g yigld lgss t.h~ n I 00%? (I)
(cf) \1\frito 'tho ion ic half-oqu~'tions for t ho rodu ction of cl"2~2:- ions in :lcid solution
to Cr3"" ions. and c r3+ ions t o c rZ• ions. (2)
(e) Why was t:he screw cap left open unt il t h e solu t ion went blue? (I)
(f') Why d o the chromium(11) ethanoate complex and 'the hydrated c hrorniurn(u) ion
have d iffet"'e n ·t colo u r-s? (I)
_..
Makta surQ that your yield is >SO%. • Make sur e that you Kn ovv how to m9asure l"'''lQit lng
R.Qm Qmbert.o rQCord a ll rn.a.SSQS t o 0.0 1 g. t.Qmpe~tu i"QS a.nd how to rec:ryst.alllse a solid .
all volu mes to I ~m, and melting temperatures • Rec:ord 't:he shape and ex>lo u r o f an inorganic
"'to I °C. product.

EdeXC:QI A S/A2 ChQmlstry

 Questions & Answers
T h is section conta i ns exa rnpl es of the type of experiments a n d questions that you wil l
e n counter In Acttvfttes B . c and o tn your Internally assessed practica l tn Units 3 and
6. It also contatns the answers to these Test <:~uesuons. A liCk (.,....) represents a scortn&
poJnl.

Test questions
AS questions
Ask your teacher tr you can do these exper tn'lents. The ide n tity of the unknowns and
the concentrations or solullons are Qlven tn the answers. whiCh follow each <:~uesuon.

YOu must ask your teacher to carry out a riSk asscsstncnt before doing these experiments.

• ..

U ntt 3 and 6: Chemistry Labor-atory Skills S7

 Question ,. & An10wer·s

Tesc quescion
Carry out: t:he following cescs on che cwo solid inorgani c sales. A and B . and a solucion of a111 ino r-gan ic sale. C.

(a) Cal"'ry out: a name c.e:n : on solid s A and B . W ri t:e down your o b servac:ions with A and wid'\ B . (2 markS)

(b) M a k e a solu don o f son"'e o f A in 3: crnl. o f wa.cer and add 4 drop~ of dilu~e hydrochloric add.
f o llowod by S: drops barium chl o rido solution . Writ:o d own your o b sorvat,ions. (I mark)

(c;) U sing your obsorv:ations i n ('!') and (b). i d CIIntify A by writing its formula. (I mark)

(d) Write the ionic equacion for t:he react ion observed in (b). (I mark)

(e) Heat: some of solid B in a c:est: tube and pass t:he aas evolved i nt:o lin11ewa.cer. W rh:.e down your
o bservatlo•'los. (2 markS)

(:::# T h ere are 2 mark s . so t.wo observation s m u st be m ade.

(f) H eat: 3 crnl. of wat:er" in a cese c u b e - ahnosc co b oiling. Add some solid B and c:e.sc: any gas
evolved wit:h lirncwat:er. Writ:e down your o b ser-vat:.ions. (2 marks)

(a) U sins your obsorvat:ions i n (a). (o) and ( f) . writo tho formula o f B . (I mark)

To l; c;rnl of tho solution of C, add 4 drop:~~~ o-f diluto nitric 9c;id, followed by $ drops o f aqueou:~~~
silver nitrate. "rhen add aqueous anunonia unci I c h ere is no f"urth er change. W rite down your
ob,ervat::lons. ..
(l) To a second 2 cml portion o f aqu eous C, add I 0 drops o f dilu te sodium hydroxide s .olution.
Writo down your obsorvatiQn$. (I marS<)

( j) U sing yQur observatiQns in (h) and (i), writ4 t h e f"o rrnola of C. (I mark)

Toea I! I 4 marks

Tesc quescion I answers

A IS potassium s u H~:ne; a IS sodium hydi"'Q:encatbonate; cIs a sotutton or rnaQ:nestum
chloride
(a) A gives a lilac V' name colour, B g tves a yellow V' colour (a llow ora n se)
(b) W h ite precfpttate V'
( c ) K 2 S04 ...-
( d) Ba2._(aq) , S 04 2 - (oq ) - BaS0 4 (s) ...-
( e ) Drops of water condense ...- on upper par-t of test tube; l imewater g;oes milkY ...-
(f) Fizzes ...- as e ts added; limewater goes m ilky .,
(g) NnJ--lCO~ ...-
( h ) Whlt.e practp1tate v w hic h d is~ol ves in a mmonia solution V'
( i) White ptectpttate . ,
(j) MgCI2 ...-

58 Edexcel A S/A 2 Ct"'QI'r"''i stry

 Test estlon

T est q u estion 2
Carry out: t:he f ollowing: cest:s on chr-ee Ot"8anic compounds. P . Q and R.
(a) M ix I crnl aqueous pocassiut-n dichr-on'l!ate(vl) and d iluce sulf ur-ic acid in a c est: cu b e~ and add
S drops of P . Plac:.e t:he t:est: cube in a beaker of warm wat::er for a few minut:es. Wrh:e down
your obsorvat:ions. ( I m nrk)

\,:* Record 'th e colou r befo•-e and after the test.

(b) Working in a fun"le cupboard. put: I c•n:J of P in a dry test: cube. Thet"l carefully add half a spat:ula
of pho.sphorus(v) chlor ide. T ost: t:ho gas evol ved wit:h damp blue l itm u s paper. Write down
yovr obso r vat:ions.

(.::* T ker-e are 2 mal"k.s. so t \1'\1'0 o b sei"'Vations n"\ust. be mad e .

(c) L ook at: t:he mass spect:ru rn o f P below.

f
• j ..

By considering your answer's co (a) and (b) along w ich t:he 1nle val ue of t:he molecular ion
and the f ragment: ion at: ~~n/e - 3 I i n the •-nass spec::-t:rum. w r ice che f ortnul a of P. ( I rn&.rk)

(d) Pour 3 c~"l o f aqueous s ilver n i t:ratc into a t:ost t:ubo and add 4 drops of Q. Then add aqueous
a~n"'on i a until there i s no f'urt:her change. Write down your observations. (2 m a riu)

(e) The mass spectrum of' Q has two molecular ion peaks of' equal intensity a.t rn/e values of'
136 and 138. U sing chis and your answer co (d). a .'ld t:he f act: chat Q has a branched ehain.
w rit:.e a formula of Q. ( I m.:..rk)

(f) Put: a fow drops of R on a cruciblo lid and ignit:o it:. Writ:o down your observations.

U n rt 3 and 6: Chemistry Labor"atory S ki lls ,,

 Question " & An$WE!I's

~ T h ere are 2 mark s. so 'tWO observat ion s rY'I U S"t be n'\ade.

(s) Pour 2 en"lo:l o f bromine wacer in co a c:e~c c:ube and add 4 drop$ o f R . Gendy $h ake che C4'!!$C t:ube.
Writ:o down your obsorvations. (2 markc}

(h) U :fing your an$Wetrs to (f) and (g). sta~e e;h e fu n c::t:ional group in R and $UQSCt$t: another f4;u~~ot:ure
of t:h e mole cule. (2 marks)

(I) The inf rared 5pec.t:run'll below i5 c:hac of P , Q or R . Exan"line the spectrum and, using you,.. daca
b ookl ety ident.ify t::he compound which ha.s t:h b spe.et:rum. Just:ify your choice. (2 mar~)

100

1
..J so

• ~~ooo~~~~.-~-.~,ooo~~~~~~.-~,~o~oo:=~--.--.--~~,~s~oo~~--.--.--~~,~ooo~~--~--.­
wavenurnber/ cm-•
..
Total: 14 marks

Test question 2 answers

PIs propa n - 1-0I ; Q 15 2-bromo-2-n'lethylpl"opa n e: R rs cyclohexene
(a) Or-ange SOlutiOn Q:OeS gr·een V
(b) steamy fumes . , dVOived; b lue litmu s goe~ red . ,
( c:) CJ..-t_,C I--I;,:CI-I:z_OI-1 V
(rh e r-eason rs that tt ts an alcohol having: an OH gr-oup and the m/e value of the
rno teculal" for'\ ts 60. so t h el'e rnust be 3 carbon atoms (36). one OH (17) an.d 7 othel'
hydrogen utoms m.aklng 60. The peak at 3 1 Is 29 less thnn the rnolccu lo.r ton a n d
r e$u l ts f l"om the loss of a Cz ..l o group, so P m ust be CH 3CJ-t ;r_C H :~OH. n ot
C H~C H(OH) CH~ .)
(d) cream precipitat e "": whi ch s l ays on addttton of dJiul e ummontu v-
( o ) (CI b).;,CBI" O r" (CH~)zC II C I hBr V

Ede><:Cel A S/A 2 ChEHY'Ii stry

 Test estlon

@ Either of t h ese formulae w ill score.

( It l s branched (the question says so). The two peaks of equal intensity of the
rnotec:.utar ton s h ow that t:here ~re two Isotopes with equa l abunda n ce. This must
be BI' ana conrtrms me tnrerence rrom u 'e ct'eam colour tn <CI>. 136- 79 (or 1!)8- 81)
lcuvos 57 whJch Is made up of 4 cc:a.rbon atoms (48) and 9 hydrogen atoms, so Q t.s
2-bro n'l o~- met hylpropane or 1- bromo- 2 - m eth ylpropane .)
(f) Burns with a smoky flame ......
(g) Red-brown bromrne goes colourless v (Qoes clear would NOT score); t wo layer'S .....
forn'l
(h) C=C (a l kene) arol.I P V'; a hiQh car'bon-to-hYdrog:en ratio v
(i) :Specuum ts or P ..,...; b J"'ad. peak a t 3.:>~cm- • due to a h,Ydrogen-bonded 0-H grou p ..,...

• ..

U nrt 3 and 6: Chemistry Labor"atory S ki lls 61

 Question " & An$WE!I's

Tesc quescion 3
You are supplied wid":
• a saw. p i e of a solid lron(11 1) co.,...pound labelled Z
• aquoous 0.100 n-.ol drn-1 sodium thiosulfn.tc
• aqueous O. Srnoldn-.- 3 pot:assium iodide
• dilute sulfuric acid
• sta r ch solution.
lron(lll) ions reacll!' wit:h iodide ions acc ording co the equat:ion:

Tho liberated iodine can bo titrated with aqueou s sodi un--. thiosulfatot
h(aq) + 2S20l 1 -(aq) ~ 2 1-(aq) + s .. o.l-(aq)
( I) Weigh the weiahina bot:de cont:.a.inina z. Copy Table I below and record t:he mass of t:he bottle wit:h 2..
TAblet
M ass or weighing boc:c:l e wlll!'h Z /g
M ass of e~ptl ed welghh'lg boccle/g
M ass ofZ/g
Tip the solid Z into a I SO cmJ: beaker and reweigh the bott:lo. R ecord tho mass of tho empty bott-le in
t-ho t:ablo. Thon dissolv.;, Z in wator. t:ransfCIIr t-hea. solut-ion into a 2SO c m 3 volurnotric flask nnd n-.akQ it up
to the mark with dist:illed water. Shake the fla.sk c h orough ly.
..
(3) Rinse out: and t:hen fill a burec:t:e wich t:he sodium t:hiosulfat:e soluc:ion.

(S) U sc measuring cylinders to pour 10 cml of dilute sulfur ic acid Qnd 10 cml of potassj;um iodide solution
int:o t::hq, cc:tnic..--.1 flask.
(6) Tit:rat:e the solut:ion in the conical flask wit:h t:he sodium 't:hiosul-fat:e solu-d on unt:il the col our has faded
c:o pale yellow. Then add I 0 drops of search indicacor and concinue co add che sodium t:hiosulfat:e drop
by drop until the blue- black colour has disappeared. R ecord your burette readings and t:he t:itres in a
tablo (scto Tablet 2).

Tlt:raclon number I 2 3 4
Burecce readln$1 (flnal )/c:rnll
Buren:e reading (lnft:Jal)/cn...ll
Tlcre/ern'

(7) Repeat steps 4 - 6 until you obtain t-wo consiste nt titrc:s.

List: t:he titros you will vse t:o cA i cvlatt;t t h o mct::an titr-e.
Writ:e down t:he mean t:it:re (cml of O.IOOrnoldn,.,-3 sodiu•n t:hiosul-fac:e). ( 10 mar ks)

62 Ede><:Ce l A S / A 2 ChEHY'Ii stry

 Test estlon

(a) Calculat:e t:he amount: (in n"'loles) of sodium t:hiosulface in che

mean t:it::,..e. ( I mark)
(b) Using t;h q oquat:ions giv4n cu ;artior And your g,n s wor t:o (a), c;a l culat::o
che amount: (in moles) of F e~ • ions in 25 . 0 crn"lo of solucion . a.n d
hence in 250crnl o f solut:ion. ( I mark)
(c) U sing you..- a n swor t:o (b). calc.u l ato tho mass of iron in 2S:Oc.rnl of
solution . (A..(Fe ) - S$ . 8) (I mark)
(d) U sing your answer co (c) and t:he tna3s of Z taken. calculat:e t:he
pcr c.o n t .ago of iron in compound Z. ( I rna.rk)

T ot:al: 1• marks

Test question 3 answers

z fs hydrated ammontun1 lron(m) su l fate, ( NH4 hS04 . Fe;a.(S04 );,.24H 2 0
samples ofZ s h ou ld be between 11 . 2 and l l . SQ in a weighing bottle
The sodium thiosu l fate solutton f s O.IOOn-.oldn'l-~

scoring
• Table 1: all masses to at least 2 aeci m al places and subtr-action correct ..,...
• Table 2: all volumes recotded to o.oGcm3 and a ll subtracu ons correct ..,...
• Mean titre: correct ly calculated ..,...

• • Accuracy m a rk: the expected titre - m ass of z

Differ ence f"rorn expected th:r e

:w 2 . 074cm~

;t;O . ~ ;t;O . S ::t0 . 7 ;t i .O > 1 .0

..
M arks scored 4 3 0
consistency n1arK.: difference between outermost tltres used to ca lculate the mean

I D ifference
M arks scored
I0 .2
3
I~.3 I~.s I~o.s I
(a) Amount orsodtum lhJosu lfate = o.toomolctm- , x mean tnre dm,..,...
1 000
( b ) Atnount of J2 - Y.a )( n"loles of sod ium thiosulfate
Amount of Fe 3 ._ tn 25cm:') =
2 x m oles of 12
Amount or Fe 3 ~ 11, 2.50cm 3 = 10 x moles of Fe 3 + an 2~cm 3 .,...
(c) MU.SS of I r o n In 250cm3 - 55.8 M O"lOICS of Fe:>• In 250C.n"l3 .....
(d) 96 iro n In Z ... mass of iron rn 250cm3 x 10096 ..,...
mass ofZ

U nrt 3 and 6 : Chemistry Labor"atory S ki lls 63

 Question " & An$WE!I's

A2 questions
Ask your t eac h er ff you can do these experltnents. The idenUty of the unknown s and
t h e con centr-ations of soh,ttion s are g tven tn the a n swers, whrc h follow each Q1.1estion .
YOu must ask your teacher to carry out a risk asscssrncnt before doing these cxporlrncnts.

• ..

Ede><:Cel A S/A2 ChEHY'Ii stry

 Test estlon

Test question 4
You arc;t supplied wic:h c:hree cu··aanic: c.ompounds X , V and z . each containina four ca,.bon atoms. Non e of
che con'llpounds has a branched carbon chain.

(a) Look ac the spect::ru"" of X below and cotYU't"'lenc on che inforn-1oacion chac chis provides. ( 2 m a rkS)

so

0 ~~~~~~~~~~~~~~~~~~~~--~~~~~~
4000 lOOO "l(X)() 1500 I 000
Wavenumber/ em-•

• (b) Make up a solut:ion of equal parts of aqueous pot:assiurn dichrornat:e(vl) and dilut:e sul-ful"'·i c acid •
Divide chis lin co t:hr"ee in chree separac:e c::esc: cubes. Add 4 drops of X to one,. 4 drops of Y co an ocher
and 411 drops of Z to t:ha third. Warm each in a beaker of hot watc,. for 3 minutes. Write down your
..
obse t"'Vadons wit:h X. Y and z. (3 m af"'kSS)
(c) Add S drops of 2.4-dinit:rophenylhydr"a:z.ine solut:ion in t:urn to X. to V and c:o z . Wrice down your
ob-servatiions with X . Y and z . (3 marks)
(d) Make up a. solution by ad dins aqueous iodine to about IOcrnl of dtlute sodium hydroxide unt:il t:here is
A faint brown colour. Pour equal arnovnts int.o three te5t tube•· Add 4 drop• of CH11c;.h of X . of V 3nd of
Z to che separace cesc c:ubes and allow c:o s-=.and for" 3 rninut:es. Wrice down your observations wich X. V
and Z. ( 3 ma•'i<.S)

(e) ldent:ify X. V and Z by narno or for,-,ula. ( 3 m a r-ks)

Tot:al: 14 marks

U nrt 3 and 6: Chemistry Labor"atory Skills

 Question " & An$WE!I's

T esc quescio n 4 a n s w e r s
X I S butan-2-0l. C t-1 3 C J-t(OH)Ct-1 2 CH,:,; Y f..S buta1'1a l , C H ~CJ-I 2 CJ-t 2 CHO; Z I S butanon.e,
C:IJ~C:C>CII2C:I I ~

[If thct·o Is any troub le gcttl ns hold of these substances, the p•·opan ... equivalents ca n
be used .)
(a) Has a n 0-H aroup V'; but no C=O Q:roup .,.... (This means t h at u Is a n a lcohol )
(b) W i th acldlCie d d f ch t·omntc.(vt):
X - or::a nge solutton goes green V' (Thts m ea n s that X I s o prtn'l.:lry or secondat·y
alcohol- see (a))
Y - oranse sotuuon s_oes Qreen V" (~rhts means that v Ls a primary or secondary
alcoh ol or an aldehyde)
z - soh.tt1on stays ora ng:e ..... (Z rs pt·obably a tertiary alcoh ol o r a Keton e)
( c) With 2.4-dlnl tr'Ophenyl llyCII'aztne solutton:
X - no proctpllato . , ( I t Is n ot a cnrbonyl compound)
v - yellow (o r orange) preclp lt;::~te I s fo rmed . , (It I s a n aldehyde - see (b ))
z - yellow <o,. o ..anae> p.-ectpltate I s formed .,. ( It rs a ketone- see (b))
(d) 1n the Iodoform l est:
X - pa lo yel low p t·eclplt a t e . , ( It contain s CI-I ~CI-1 (01-1) group and so Is butan ..2 - ol)
v - n o precipitate ...,... ( I t Is butanal: It ca n not b e rne thylpropanal because that h as a
b.ranc11ed chain -see sten1 or questtot1)
z - pule yc11ow p t·cclplto.to V" ( It contains a C J I ;,CO group, so l5 butanono)

• (o) X I S butan- 2 - o l , CH: 3 C l-I(OH)CH 2 C l-l;, V ; V t s but::.na l , C I-I;,CH 2 C l-1 2 C H O V ; Z I !to

butanone, CH 3 COCH 01 CH 3 V ..

66 Ede><:Ce l AS/ A2 ChEHY'Ii stry

 Test estlon

T est ques tio n 5

You a,..e given chree solucions c.oncaining three differ·ent: salt::s- A. Band C - o f d-bloc.k rnet:als.

(a) Wrice down t:he co lou,. of each soludon. ( 3 markS)

(b) To a pordon of solut:ion A. add a•n•nonia solution until in excess. Wrilce down your
observations.

(c) To a soc;ond po,..tion of solution X. add I c:rnl o<f diluto hydrochloric acid followod by
I crnl: of barium chlo.-ide solut:ion. Wrice down your" obser"vat:ions. ( t mark )

~ Record 1.he colou r oft:he pree ipitate and not. ·the solution a_bo,.;e i t..

(d) I dentify X by writing iit:s formula. ( I m a..rk)

(o) To separate portions of solutions B and C~ add aqueous sodium hyd..-oxido until in cxc:oss.
Write down your obse rvat:ions wit:h B and with C . (3 markf:)

(f) To a seGOnd po,.t:ion of B . add 5 df"'ops of pot:assiurn iodide 5-0i ucion followed by 5 drops
of st:arch 5-0iue:ion. Wric:e down your observacions. ( 2 maM<.s)

• \ J Rooe:on::l 1:h o colour :afto.- :addinsz pot:;;assiu i'T'\ ioclid o a n d :.fuw addina st;;an::h.

(a) Identify the cation$ pna$e nt in 8 and C by wricina their f"ormula.e . (2 m arlu)
..
Toca.l: 14 m a rk$

T est questio n 5 answe rs

A Is a solution o f n lckel (u) s u l f ate; B ts u solution of rron (111) c hlo ride; C I s a solution o f
c hrornh,.a m (rn) sulf-ate
(a) Sol uUon A ts Q:l"eeo ..,...; s fs ye llow-btown .,....; c Is Q:l"een ..,...
(b) c.ree.n prec tpnat e ,., fot'med: rorn1.s a pa te b l ue .sotuuo n wnh excess .,....
(c) W h ite p r eci pitat e ,., form ed (not e t h at It ts n w h ite precipi tate I n n s •·een sol u tio n )
(d) NIS0 4 .....
(e) e - red- brown ptectpu a t e whte h s tays with excess v
c - green p r eci pitat e """': fo t·ms a s •·een sol u tio n w i t h excess .,....
(f) B g i ves a r ed- b r own solut io n V'; goes blue- b l ack w h e n st.;;~; rch ts added .,....
(g) I n B IS Fe;,.. V'; In C IS C t.3• V'

U nrt 3 and 6 : Chemistry Labor"atory S kills 67

 Question " & An$WE!I's

Tesc quescion 6
( I ) Use a mea~uring cylinder t::o measure 30em~ of I . Omol dm - :J sulfur i c acid and pour it: int:o a beaker.

(2) C lean some masnesiun"'l ribbon wiith sandpaper and c ue: ic: inco 4 e qual l e n.gt:hs bec:ween I a nd 2ern.
(li) Measure c:ho t:cn,pcrature o f t:hc a c id . The n add one l e ngth of magnesium ribbon and st:art: a c loc k.

(4) St:op tho c l ock when t-he rn~anosiun--. disappoars.

(5) Measul"'e out:. a.not:.her 30cml: o f acid a nd war•n it: on a t:.ripod and gauz.e unt:il it:s t:e•nperat:ure reaches
just: under 3oo c.
(6) R o rnovo fr o m tho h o at:. m oasuro it:s t: omp o r~turo o::~nd add " pic;tco of nuaanosiurn ribbon. Tirno how l ong
it: c-akes for all t:he maJilnesiurn t:o react:.

(7) R e p eat: st::eps 1-6 at: 40°C and 50°C.

(8) R ecord all your lflea.su re.....,ent:s h 'll a cable (see T a ble 1). (2 markS)

(9) Copy and eo""pl ec.e T abl e 2. (4 mark$)

1 -E.
You may o::~ssurnc;t thAt l og 10 ( -) i s proportional to-....:;.:_-. whc;trc;t t is thc;t tirno. Tis t:ho tomporat:uro in
t 2.3RT
kelvin and A - 8.3 1 J K-1 mol-• .
J.. o n t:he .x-a...xis.

•
(a) Draw a g raph o f log1o(..!..) on t:h c y-a..xis agains t:
< T
(b) Ca.lcula:t:e t:h e slope of t:h e graph. S h o w o n the araph how you did chis.
(c) Calculat:e t:he ac.t:ivat:i o n energy f or t:hi.s react::ion. Give a sign and unit:s wit::h your answer.
(4 marks)
(I mart()
(2 markS)
..
(d) Suggest: one rna in ~o ur ce o f in accurac y in t::his exp e rime nt:. (I ma••k)
Tabl e 1
Volun, lliil of a.cidlcrn3 Lenat:h of n,aa:nesfum/cm

Tabl o '2

- 1-ls- 1
• l os,cr-L
• T e m p e r a.t:\..lre. T/ K +/K-t

Tot:o::~l : 1... rno::~rks

68 Ede><:Cel AS/ A2 ChEHY'Ii stry

 Test estlon

T est q u estion 6 answe r s

Table 1: AU volumes .,..... and u mes v recotded
Table 2: correct calcutauon or: +
v ; I O.Q 10 + . ,. .: Kelvin Lemperature v ;
(a) Craph : sensible sca l e a n d axes labelled V ; points prope r ly p lotted a n d best- nt
~ .,

stta&ghl llrle drawn .....

If all potn.ts c lose t o the line ..........: tfonly on~ S l ~n sn cant ly ofT the Jtne . ,
(b) Slope ca le u lat.ed properly . ,
(c) Activation ener~y =(-slope,... 2 .3 x a . ~ I )+ 1000 kJ mol- 1 : va1-.1e .,...; s tgn and correct
un.Jt .,....
(d) Either tho temperature was n ot con su:tnt during each experiment: or the places of
m agnesi u m were n o t of exactly the sam e length . ,

• ..

U n rt 3 and 6: Chemistry Labor"atory Skills 69

 Knowled check a n s wen;

Knowled e c h eck answe•-s Tho rno/os ofhydrochloNc Odd oro rnutupf1od by ~ to gcK tho
tnOklt$ o($Or;IA,Jm <;arbonote be~covs:o thoro ts I Na;zCO~ to
(a) Lil.2c: fbrno V' 2 HCttn Che equouon. rn:us
(b) Drops of water condense in upper part of "ten. tube ...-": t.he (~) Mol011r- IT\0\S$ of~h• l"lyd r~ted sodi~,~r-n c.011rbon aw = rnoiiS
lirnew.:n_e,.. a oes m ilky V' 4 .1 1 a r-no
(c) The solUtion suys dear and colourless .,.... - 0.0144 m ol
(d) KHC~ V' - 2S5 g: rnot- 1 V"
2 (411) Forms t."'-"0 la.ye•-s .,....: the univer~.l indicator ~oe s areen V' (d) N...-nber of l"nOiecules of waur of crys~alltsa~ion i n
(b) Steamy fumes produ ced ....-: litr'i"'Us paper aoe5 r"ed V' N.:."2C~.xH10.
(c) The so'-rtion 'tlY$ or.anao ...,... mass of xH,O = 295 - (mass of Na-,.CO~
(d) The peak at P iS caused by t:he 0 - H bond V' and the peak - 2 8 5 - [{23.0 :.< 2) ... 12.0 ... {3" 16.0))
at 0 by a c-1-4
bond V' = 17'9.0
x = 179.0sz
(e)~ ., =9.9
I S .Oa

So mere are 10 molecules of water of crystallisation ..,..

:1 M01.ss of solid - :2.-4.16 - 23.25- 0.9 1 a I I I n"'O I o f C r -,.0 7 2- sz:i ves, 3 mol of 1,. wl"li c l"l r-equ i re 6 .....-.ol o f
Error 's : 0.0 I per r eading. so ± 0.02 520~'2-
2
Percentaae error= ~;:! x 100 = :t2.2% So ~l"le r~tio of S-,.~2- ~o C r-,.e>y2- i s 6: I
12 (a) Nu-nber of moles of sodium ~hlosu l fate In the mean t.ltr'e
4 The masses shoul d have been recorded t.o 2 dedmal ptace:s. - conc;er"Ttr-a~ ion :oc; volu!T\8 i n dm3
S: In titra:tion I , a full burotto has a road i"''l oro, not: SO. - - 3 21.50 3
In titration 2. the tJtr"e and the mean tl'tt'f! shouk:l have been - O. II I rnof diTI JoC IOOO ck-n

g iven ~o 2 docim:~~l placaso, "th.:lt is 22.30 not 2 .2.3. It is accopt.ablo = 0.004397rnol V"
for an lnll;ial readfna of zero t.o be wrh:ten as 0 rather "than 0.00. (b) Nu-nber of n"'Oi es or Iodine liberated = ¥.& x 0.002387
6 E rror is~ 0.05 perro.:..d i ~ so±- 0.10 in tit.re =0.001193 .....

• P erc:enuae e 1'T"Or- i~ ~~~~~ " 100 - 0.~5~. which is mucl"l I•~~

1t"lan tl"le percent.aa e error- of 2.2~ i n 'Weig:l"lin,a, {Nou.: 'tl"le
major e l"'t"'Ors. due 'to apparatus. in A-le~o~e l measurements are In
Nu-nberormolesorMI ~ In 2S.Ocmll = Y) x 0 .001193
= 0.0003979 ..,.
Nu-nber or moles or M t O:l ln 250crnll = 10 x 0.0003978
= 0.003979 V" mass
..
weial"lii"'IQ: o r in usinsz: Ol l:herrn Qn"leter or measurina cyli nder.)
7 M otes= concentration x volume In dmll = O.l23mol dm- ll
(C) MOlar mass of M l 0) =
iTi'O'iO'S
x 0.023o45 drnl = 0.0029SI"n01 o.s.s a
0.00147mol 0 .003979.....-.ol
8 Concent:ratJon = moles/Volume In dm3
- 0.055"' mol dtn-3
0 .0265"' drn)
= 2 13 .7 arnol- 1 ..,...
9 A.r'nOu'"tt of sochum hydroxide in the mean titre (d) A,.orM = 213.7- ( 126.9 + 3 X l 6 .0))
2 1.90
-O.I I In"lol drn-3" IOOO d1"n3=0.002431rTiol V"
= 39.8
The aroup 1 metal M Is potassiur'rl (relat.lve at.omic
AfnOU'rt orH 2 X In 2S.Oc:mll of solutiOn- J..'!r x 0 .00243 1 mol m~ss 39.1) V"

= 0.0012 15n"lol Look (br Che e~ whOse ocotn~e moss IS dosest co

The l'l"tties or
sodiUm hydt"'><H:Je o,-e muluplled by¥.& to get the yovr om~r. Th9 c;llft79ntfll"l<» bot'W9erl tho t"'-'0 Is
expenrnent.ol error.
~ousod by

moles o( H 7 X because there IS I H,X to 2 NoOH m the equoUOI"t. (e) Tl"le ~lution in the buret~• 'WOUld h;lve been m ona di l u~e.
Henee. tl"le .srnou nt: of H:z.X i n 250cm~ or so'-stion so mo•-e 'W'Oukl have had to be ••un In .-'
= 10x0.00121Smoi = 0 .0 121SrTioiV" 13 (a) N...-nber- of l"nO i es of sodi un"' ~l"li osu lf;tte in V"le ~T~ean 'ti~-e
The mol ar rn:!l.Ss or tl"le a.eid H 2 X - mas~ of H 2X usedlan~r = concentrat.ton "'volume In dm,
1 53 _ _ 26AS
&
to (2)- O.O I •2 15mol - 126a m o l - 1 V" - O.II I moldm 3 x dm-3
1000
I 0 ( a) Amount o f I'Tydn:>chloric acid i n 'the mean ti1:re = 0.002936mol V"
0.123rnoldrn-l x 23 .45 dm3
= (b) Nu-nber" or mol es of iOdine. 12 - Y.t "' 0 .002936
1000 = 0.001469 .,..
= 0.002894rnol V" Hence l:t'le amou i"Yt or h)'droszen pef'O>ode in 2S.Oernll
(b) Amour"'t.Ofsodiumearbon.rte in 2S.Oc:r"'Y - }'!rx 0.0028&4mol
= 0.0014421T10f .....
Hence. 'the amoum In 2SOanll = 10 x 0.001442m01
(C) ~~~~::'n°~;"
0.0014691"nol
me hydr'Oa en peroxide solutiOn - ~::,s.
- 0.014o421"n01..,. 0.
0250
d,.,J = 0.05872 mo l dm~ ..,...

70 Edexcel AS/A2 Ct"'QI'r"''i stry

 Knowled check t.r ,swers

{d) Amount ofo)o()'a:on produced=~ :oc 0 .05872rnol ( b ) T .......o rtra.iaht l ines drawn And ~ra.po l.s.ted .....; from ara.ph:
= 0 .02936mol oT = 9. 6·c ~
Volurno o f CO<)"Ven produc.ed = 24drn.lrno l- 1 :roo 0 .029361'"1"\01 accuracy vAlue zo.s•c .,.....,....~ :Lo •c .,.....,...: ::1:2.o•c .,....
= 0 .70Sdm:. or 70S em:. .,..... (C) Heat ct'lanae = mass of solution x spedTec heat. capaci'ty x o r
14 Polystyr"'eno is a muc.h ........orso c:ondu ct.or o f h o.:..t than &~as:, and - 2s.o 2 • .... ISJsz-'•c- ' JOt 9.6•c
so less heat will be los't 'to me surround~s and the expe riment Make sc.v-e you use
the moss ofsoJuuon not the moss of 'Che
will bo moro ac:c:ur.:..u:.. %Inc when eolculoung the h~t c hange.
IS (a) enef1ZYtransf'en-ed = mass ofsol ut.lon x 4,1SJrr '•c-• x 6T = 1003)
'"'"'2S.Oa :oc <4.1 8Jg-'oc-• x 7 .7°C - 1.0031<,1 ......
= 90S J = 0 .80SkJ .,..... (d) Amount of copper(li) sutfat.e = O.SOO~n04 dm -s x 0 .02Sdm -s
Moka suro that )'OU uso tho t ncus oftho solutiOn (25B) and - O.O I25 mol.,....
not dle mass of potassium cort>onote soild token (2.58g)'" 6H = 1.0031<.1
this co/culatlon. mass 0.0 125mol
(b) Amo unt of K2CO, = mol;:uo mass = - 90.'2 4 k;Jmo l - 1
_:2".5~8~"!!....~
-138 Because t.he t ernperoture I'Ose. t::V-1 rs negouve.
_ ..., _, = O.OI87mol . , = - SOkjmol -1 .,.... for vah,.ui to 2 s.f,; . , for s ian and v n it
22 01
(e) Tl'\e soh..nion woul d become c:otour'less ....:-
al-/ 1 - - 0 .805kJ =- 43 kj m o i' V" (f) No, bec;cuo~s9 t l"l9 aiT'IOUnt o f h 9n wovl d doubl 9 , bvt so
0.0157rnol
-
.......ou ld U'le mass or solution to be neated up ~
The vafue or.OT 1s on¥ CD 2 SfgnlfkOnt f72ures and so the Tt-.vs ATvvoutd n ot 0111t9r 01nd ~the •c:c:uracywou'd
answer to 4H must also Oe to 2 s.f, The 51Qn of4 1-/ls neBQttve also not a l t.er v.
bec:ouse the c~mpe110 c.u;e rOSe. 18 ( 3) Fro m the arapn: AT = 27.4 - 19 .0
16 = 9.4•c .,....
/>.11 Votum9 o f N .. O H = 2.6.Scm 3 .,....
2Kl i CO,(•) (+211CI) K;.CO,(S) + COJo(g) + ll:,tO(I) ( + 2UCI) Accuracy o rt:J.T. : o.s•c .,.....,....~ :r1 .o•c .,.....,....: :r2.o•c .,....
~ Ac;<:uracy of ~ ho~rne: :t;O. Sc:.n3 .,....,....; :t; I.Qc;.rn3 . ,

• 2 X
.2KCI(s) + 2CO.,(S)
________-;;;,,

+ 2 11;,0<,1)
(b) To"tal volu m e = socm2o + 26.Sc.m2

(C)
= 76.5 c rn3 .,....
H eat cnana e = 76.5~ x 4.1 8J2""'•c-• x !J.4•c-•
..
Labelled diag ram ..... .,..... = 3006)
6 H - (2 w 6 MiJ -a.~-~, = 3 .0061<J
......
1
= 2 x ( + 29 k;Jmo l-') - ( - 43 k,Jmol- ) = + 101 k;Jmol- 1 .,...
(d) Amount of ~Ol-t = 2.0 r-no l d rn-3 x 0.02.65 diT'I-:l
Mok.e SUf'e thot the dtnt:cUons o(" arrows agree wtth the lobeUJng.. = 0.053 mot
For tnstonce the "'wer t1Slht-hond arro..v OtXJk:l have been drawn = n vrnberof m oSQsof HNOJI .,....
pomung up right,. but then the Iobei must be - 4flH1. - 3 .006 1<.1
17 (a) t...abe lled a.><es wi'U"'l set"Sib6e Kate and points P'otted c.on-ec:tty . , (o) d l-4 - O.OS3mol
- - 57 kjmol - • .,....
(f) No. bec.ause the volume c.annot be estimated t o better
than :ro.s c.m, .,....
' 2.24£
19 Motes of N 10 -74.7 gmo l-l - 0 .0300 r-nol - thoorotic.al moles
of n ickel sulfauo
Mohtr ~~~of N iSC>4 .6 .... 2.0- 262.8a rnol - 1
T heoretk al mass o f nickel sulfate = 0.0300mol x 262.8szmot-•
- 7.ee a
~yield -
actual n'\a.SS
tfle o ret.•c •i rT'Ias.s x -
IOO
. 2 w I
;·:a a
OO

- 72.0" or 71.99& if all f~res ar-e kept on t.he caku b :tor.

:zo ( a ) Slight ft-othinsz:""" and 1t"le solution turning: btue .,...
( b ) Some or it ..el'nAined u ndissofved .,....
(c) I f evaporated t o dryness. 'the anhydrous salt w i ll be
fo •-med """
(d) Slue .,.... and rhombus shaped .,...
(e) N umberorrnolesofacid- I.O rnol d m - :a • 0.025drn:J
= 0.02S m o l
Tfme/n·dnuces T heoretieal an'lou n' or CuS0 4.SH,_C> • 0.025 rnol.,....

U nrt 3 and 6: Chemistry Labor"atory S kills 7 1

 Knowled check a n s wen;

Thoonrtic.al rn.ass ofCuS04 .51-f'10 =moles • rnof.ar rn;u;s ( d ) Above or bel ow 'thi s poi nt. t.ho 'temper.:..t ur-o <oNOuld nat bo
= 0.025 mol • 249.6szmot-• the bolllna temperature oftt"le distillate .,....
• 6 .2.-. R V' 24
. :..ctu.:.l 1'1"'1<1SS of produc-t
(f) ~ Y•eld t.heore"Ucal mass o f product • I OOSJC:

=
s.oa a
6.242 X I
o~~
V7'0
• 8~ ..,...: + ..,....,..... fo •~ ~so~ o~ined
25
<a> Some of the satura"ted solution d id no't crystallise ..,...: or if
no solution w:s.s left 3.(-t.er cool i n a the :.ns........er woul d be that
some anhydrous s.al't was formed V
21 (a) Beeaus.e U"le acid would fi"'''tt'' up and overll ow . ,
( b) To preven't acid spray f rom esc;~~pina . ;
( C) Yes. because the Utrnu s rumed b l ue V"
(d) Poal e a..-.en V" and d i om"'Qnd shaped V"
. 2.7sa
( o) Amount Of U"''n = SS,SQ mol- 1 26 Prop.at"'-1-ol. as i'l has neithel" a C H 3 c -o no.- a CH 3C H ( C>H)
- 0.0493 mol V' IZI'*OUP
Theoretical mass of product = 0.04 93mol x 392.0amot'""' 27 (a ) Aa;vesal'\ Or'an:lle ~cipitate .....-: wl'th B the~ is no ehan2f'! . ,
- t9.33 a.,; ( b ) With A thQr 9 is no c l-lanQ:o . ,; B producos sto4ln"y fUITI9S V'
. 15.2Q (c) With A the soluti on S'tays ora~e V': B "ti.A"ns the ol"anae
(f) "y• eld-~ • I~ sQh.rtion W""Qen V'
- 79% V' ( d ) As A i5 a c::al"bonyl c::oMpound (test 1), but is not an
( a) Some of "tho ~.atu rated solution did n o't c:rystalliso .,....: or if a ldoh yclo ( n ot oxid ised in (C)) -nd l-Ias 3 c-r bon ;tt.orns
no solutbn was leh after cooling: tne ans~r woul d be tha:t (ai'ven), it is p.-opanone.. tt will have I peak . , only (b~
sorno 011nhydrous salt ~s formed ..... CH:J a roups in tl"l" s.arne onviron monQ and VIis; will not.
( a) A yellow . , (or oran;Re) preclpkaw . ,
(b) Boc:~us.e 1ho ho-:.1: pi"''duc:od woul d v.:..poi""Ko t ho w.:..tor .:..nc::l
add steam would be produced . ,
( c) The orana o solution . , turned a:reen .....:
be spli't V' ( because there a.-e no hydr"'a en atoms 01"1 the
.adj;u::.ont c_.,l"'bon)
28 (a) FIZ%es V' and whi te solid fol"n"'edlsodium d isappeaN .,....
(b) O n nao ~olution a oos. v oen V'
..
(d) tt i s a coburtess IIQUtd .....: (c) Pal e yellow prec::ipl urte .,....
( c) T o prevent~ build·up of pressure .....: ( d ) P is bvtan-2-ol (CH 3C H (C>H)CH :zCH:J) V'
(f) The reaction is exo1hermic and so would become t oo ( e ) Q has a c -o 2rou p . , (a.bso.-pt;on at 17 Jacm- ') but no
v iaor"ou s . , and 'INOul d froth up intt> 'the condenser ......: 0 -1-1 aroup ..,... (no peak above 3000crn-•)
( R) The apparatus ""'-<M.Jid be arransred for hea'tii"''Q under refluK ...-:- ( f ) The solution nays or"an.a e V'
The e-thanoic add ........ould then be di ~Ue-d o u t or the (s) 0 is buUn one (CH:JCOCH :zCH:J) V'
mi:xtui"'Ct ......: (h) With R. the solution fizzes V' and l trnewa~e.- 'tl...rns doud)" V'
(i) Frui't)"/aluey smell .,.,.
23 (~ The bromine water tum$. from 01. red-brown c:otourto
(j) E Stel" V'
col our1ess .,.... and t'NO lay er"5 fol"'t'r"'o ......:
( k ) It i s C H .,CH 2-CC>C>H, pr-op;anoic: acid .,.,.
29 Elt.her"(CI"'(H 2 C>)&J:3• T 3oH - --+ {CI"(H 2 0 )3(C>H)3J T 3H 2 o

0 ..... ...,a,.
1hen (Cr(l-l :zO):J(OH )1J ~ 3C>t-t--+ (Cr (C>H)6l3- +- 31-1~0
C>r [C'r(H2C>)4] 3 • +- 30H - --+ Cr(OH )3 T 6H20
then C r (OI-Ih -+ 301-1-- (Cr(C>H)6l3-
3 0 Elther(c:u( H20)4),... +- 2NH3--+ (Cu(H20)•(0H )2.] - 2NH . ..
then (Cu(H20 )41 (C>H):z] +- -4NH 3 -+ (Cu (Nt-ti)~(J-1,0)2]2• +-
Note chat the equation below INOukJ also be oiiCY~Nect 2 H l:0
C>r[Cu(H 2 0).J2- +- 2NH :. -+ Ou(C>t-1) 2 +- 2NH ~- + -41-1:~.0
then C u (C>H)2 + 4 N H J + 2 H 20-+ (Cu(NH3)~(H 20)l),. +-

(b)
0 + er,

Boc:au~ i't: is l ess dense 't~n w;at.er .,.,.

3 I
2C>t-t-
(a) Green crystalS . ,
(b) Wa:t.r condentoos in uppor part o f tort tube V'; t h e solid
mens ~ be-own aas evo"-"'ed .,....
( c) Blue p •-.c.ipi'ta'te .,.,. W'hic:t-1 forms a cb.1"'k b luo solvtion with
( c) To dry the cyci Ohexene . , excess . ,

72 Ede><:Cel AS/A2 ChEHY'Ii stry

 Knowled check t.r •swers

{ d) Brown col our ..... (-'t:n proc.ipiu-te) ; on addi'tion o f sun:n a Relattv. Morni c macs of M = J,o'i x 45 22.5 =
col our v
bfue~lack So M must. b e sodium (atomk mass 23.0) .,....
(o) 2Cu2-(aq) + ...1-(o:tq} - 2Cul(s) + 12 (s) ..... (allow l,_(: aq)) (c) T n. p~:oi un-t rnana a n :lte(vll) ~oJution would h:lve been
32 (a) tt is green . , n"IOre dil ute. so t.he t.itre ""-'-Uid have been larg:er .,-
( b) C 1"'0on p i"'8C:ipita-to V which -turn~ b r own ..... on 'tho s idos of 37 ( a)
m e test tube on stanch~
(c) White procipita'to V =&.
( d ) Brown precipitate .,....
33 ( a) The solu-tio n is co lourless . ,
(b) White precipitat-e .,....: whiCh forms a colourless solution .,....
w i th OXCOS:fi
(C) Whi'te pred pft.a:te .....-: w h ich forms a colourl ess sol ution .,....
w i th oxcos.s
(d) C ream precipitate .,....
(o) Sot...ltion aoos rod-b~n .....
3 4 The oxida-uon number ofrnangoanese Chan'll@S by Sand that of tin
by 2. T n orofor o thoro rnurt bo SSnl:.. ions W .very 2Mnool- io n ,
so 'that bott"l Chansze by I 0 . (The ra:tlo ofSnh to MnO,..- is 5:2.)
35 ( a) Amount of Mno.- in n-.oo:~~n 'ti'tre - concontr.a.t:ion
volume i n dms
24 05
- 0 .0202rnol dn-1-il >e ~ drnl
= 0 .0004858mol
Amount of F o 2+ i n 2S.Ocrn3 o f solu-tion
= S >< 0 .00048SSmot .,....
- 0 .002.o;t29 n"IOI
Amoun't of Fe, .... in 250cm ,_ = I 0 x 0 .002429 mo4 Tl'\e scol"'insz ror table and this al"'aPh ""-'-utd be:

• - 0 .02.<429rT~o l .,-
M ass of~· in 2SOc.m' SOlution = mol es of Fe:l+ x A..(Fe)
- 0.024129r-nol x SS.9 ;:n-.ol -•
•

•
small :rodditions. o f a l k a l i a 1: stan. a n d ciOTdt 1:o equ i va l en~
poin't ..,... and lat"Jl~!l'' addlt.ions at other S"taaes ..,...
all volurT~ os nacon:lod to ±0.05 cm3 :~ n d :~II p l-l V<11~ to
..
= t.3SS sz .,- a't least 1 decimal placl! ..,...
9\li: ron _ mass or Fe~ In 250cm~ solut.ion • pH ~lw<11ys, risin.a as a l kali a dded .,-
{ b) ... 1 00~ • sensible scate and axes labelled with poim..s propef'ly
IT'Iass of 2
plotted V'
=~
L 3ss a
x 100 ~
• steep f'lse in pH over fi i"St rewcm:3. "then an s -st'\aped
= 1 -4 . 3~ .,. c u .....,. with a n ~ IITiort verti c;tl rise ne:~ r 20 crnl followed
(C) The concenvation of Fe,... Ions VY'Oul d have been IOY'Io"f!r. by nauenlna orr towards pH- 12.7 ..,...
nasul1:ina i n a ~rna llor 1:i1:r o V. ( b ) 20.0cm._ (v:tl uo f i'"OI'TI 19 to 2 1 .,...,...: from I 9 1:o 19, or
This wouKI mean tha:t the amoun't ofF~ ... as cak:ulated 201021.......,
would h:lvo boon l o~s a n d ~o U"le ~would nave boen l ess .....: pt-1 - 8.7 (~luo fron-t 9.2 to 9.3) ..,...
36 (a) Amount of Mno._- in mean titre = concerrtratlon x (These are the vol ume and pl-l at. hatt\ovay ~ the a lmost
volun"lo i n drn3 ven.ic.a.l p~rt) 2.0 0
= Q,0202molctrn- :3 X23
1000
65
- - ' - dm> (C) Amount o f alkal• = 0. 1 2Smo l dm-~ x
1 0
dm1 ocJ
- 0 .0004777 m o l V' - 0.002SOmol
Amount of C 2 o.
2 - in 2S.O cm:3 of solution which equals the number of moles of I-IX ..,...
- SJ2 x 0 .0004777mol
Conc:en'tr :ro1:ion of I-IX = mole~ of HX
= 0 .001194 mol ..,... volum e
Nurnbor ofrT~o l os ofC,_o.:t- i n 250c, l of sol ution - O. I OOrnol dm-3 V'
= 10 x 0.00119 4 mol (d) pH a'l 10cm:3 added= 4 .8 .....:- hence PK.. = 4 .8 .,....
- 0 .0119-4 ...... Thts Is bocouso whon half of tho acid has boon noutro/tsod tho
( b ) Mola r mass = ~~=5 concencrouon orme octd Js r.he some os the concencrouon or
1.59 @ the salt. But K.o - [H"")/fiol(} and [salt} - 1. so
[00<1) [o<Jd)
0.01194 fnOI
= 133 a:mol- •v
I<.. = (~]. and pK.., =pH.
(e) K..- 10-..~- 1o-•a
Rebtive ~:tor-nic m~u of M :x 2 - 133 - (2 x 12.0) - = 1.6 X I 0-~ (mol drn-3:) ......
(4 x I 60) = 4 S.O

U nrt 3 and 6 : Chemistry Labor"atory Skills 73

 Kn o wl e d c he c k a n s wen;

(f) Bcrtwoon pH 4.5 01nd 5.2 V' ... o (a)

(II) It Is not n e a •·l y as accura'te because It Is d iMcu l t to read 'the
vol umo ;~.1; h.:llfway up the v.nic:al p .an wi'th ;~.n .acc:u ra~ .f:1K-•
better 'than ± O.Scm:t .,....
:18 5o 'th at: 'tho values o f [prop.1.nono) and [ac:i d) alto.- by .:ln
insia:niflcant amour'l't. as 'they are much lar"Sler than ( Iodine). T his
IT"'0.1.ns 'tha't tho only v.1.ri abl es. ant 'tho conc:on 'tr01'tio n of iodi ne
and time.

,<•>
:19
-.,!:
Jt
!
S e n sible sca.le ~ points p'otted c:or ..-e-c:tly ~ bes.~frt S'tr.aiaht
l1ne dra-wn .,....
(b) Bec:a'-'$oe 1/ti me ' ' p.-cpyni on01l t:o tho r au, 'tho lo a o f 'the
rate Is p roportional to T .....
1.86 (: 1.40)
(c) SlOpe
(0.00330 0.00310)K"" 1
Th--n efmln - OA 6
0 .0002K"" 1

• The scoring woul d be:

•
•
Tabl e o f volu mes: a ll volumes o f init-i:ll sol utions
Tabl e of 'times: all trtres t.o I decimal place .,....: and all
~
= -2300K V"
(d) E .. =- slop o x S.31 J ..:,-• rnol ' ;,oo; 2..3
= - ( - 2300K x 9.31 J ~' mor • x 2..3)
..
'times to nearest. minu -te ~ t.i tres deereasina ..... = ••3960Jrnol 1
• Axes labelled and reasonable sc.aie .,....: points p lotted = +441<,1 IT"'OI- ' V"
c:on-ec:tl'y and best-fit straial"rt 1ne dr"<1wn .,... V~ l uo in ,--_,na o 39- 50 ..........; w i'th in 1-ang:o 3.3- 55 .....
,A.ccuracy of iZraph .,.....,....
• (e) Because the reaction Is e xothen-nic .,....
. ( 18 - 4)CJ"T''.l 4 I (a.) l't i s a w h i te, s.tiahtly c:...-yn.allino sol id .....
(b) Gr~d •ont = ( 25 5 ) min (b) Amoun't of 2.- h)"CCroxybenzoic acid = mass/molar mass
:a 0.70ctn3min- t.,.... 4.00a
(e) It is proportiOnal to the r ate or me reaction .....:' 138.0g:mol - •
(d) Tho volume o ftl"liosutf.a:to is proport.i on~ l -to 'tho = 0.0290mol V"
concentratiOn of Iodine in 't-1'\e sam pte removed .....-: It Is zero Theo.-etieal at'I'\OI.JI"Yt o r a.spil"'in - o.0290mol
o r der- ..... boc.aus;o -tho ra:to of ro.action is conn-ant V. Theoretical y iel d = n umber o f rno~ x molar rn;t$S
(e) So that. the concentration of propanone does not_ c:hanae - o.0290mol x 1eo.oa •"nOt-•
sian i fic.aiTtly during tJ'"Io oxpori n-~ont
.,... = S.22JZ V'
(f ) Because you do not need t.o know the exaa amo~..nt.s of eaCh (c) E lt.her because the t"eaC'tion was n01. c:ompl~ or becau$e
i2S the ordclr ofr-o::IICtion IT"'US't bo i2 whole numb o t·or- z.oro ..... some -.spim was k#t dissolved i n the water du•·il"l&
(g) The soch._..,... hydroaencarb-onat.e neutralises the acid catalyst p u l"ific.a:tiOn .....
.,....; ;;~~nd ~stops tne re.:lction ..,.., othoi"Wis.e iodi no would b e (d) So that 'the 'ternper~ure me~.s.ured • n d that of 'the sol id in
u sed up by 1he p-1-opanone du•"'nJZ me tltration .,.... the tube & 1-e the same V"
(h) The rnixturo of p .-cp.:lnono, iodine ..:lnd rtron a: .:.lk:lli woul d (e) l mpuri'ties that are i n sol ubl e in Mot wa'ter V"
produce a preciplute oftrllodometnane (&odoforiY'I) .....: ( f ) l mpu l"l't.ies u-.at. are 501ubl e i n c:old water .....
(I) Doublo 'th o c:on c:ontr.1.'tion o f prop.:ln o n o :..nd ~• h ow 'tho (a) MQthyl 2-hydroxybenzoat.e (oil ofwintef"'il•·e-eri) V'
sl ope atters ......-:- If It also doubles, the reaction Is tlrst order 4 2 Theor-etic al moles or p .-odu et = mol es o r salic.yllc a dd
with ,.. spec:'t to prcpanono .....
'"
13S.o a rnor-l = 0.007'2Smol

74 Ede><:Cel AS/ A2 ChEHY'Ii stry

 Knowled check t.r •swers

Thaorotiell ~~s o f pi"''duct = 0 .00725 n-.ol X I 90.0 a rnor-• Theore'tic~l .:arnoun't. o f [Cu(NH i).)S04 = 0.02.40 mol
1.30g Theore tical mass of [Cu(NH a).JSO.. = moles x InOla •· mass
"yield - ~:~~ )( 100 - 73.1"
= 0.02.4-0rnol x 227.6 a rnol-•
= S A 7 sz., A llow 5.46
4 3 (a) tt Is a white solid ...-: 4 .6a a
{ b) M~ss o f .-ne'thyl be nzo~:t.e = volume ~ density (d) n yletc~ = _ a )( •009€ = ~ .,
5 47
= s.oocm;, x 1.09 szcm- :a (e) Liaand exc:hang:e .,.....
= S.4S a.., (f) Some of the product st.:..yed d issolved i n 'the .:.queous
A ITIOUrrt of n-terthyl ben -z:o;rte ""'''
mol ar IY\3.SS
(g)
solution V'
To d i ssolVe the wat.el" cau sinsz the c:omplex to pl"ec:lpita:te V'
_ S .4Ssz
- 136.0a .-nol-i (h) To remove dissolved impurities V"
= 0 .0401 .-nol .,.... 45 ( a) Amount of sodium dk:hr'On'\.llt.e(VI) - mas'5/I'T\Oiar IT'I&Ss
Theoretical number of moles of methyl 3 ..n rtrobenzoa-tc - _ 2.22a
0.0401 ITIOI - 262.0arnor 1
Theoretical ITI.:ts~ o f i'Tlet.hyl 3 ·nn:roben.zo::~~te- moles x = O.OOS47mol
mol ar mass Theol"'e'tic:al amount of c:hi"''f'T''i u m(•i) e 'tl"\anoate
- 0.0-401 mol ... IS LO a rnol-• = 0.0084 7 m oi V"
= 7,25 g V" AIIOON 7.26 T l'\eor'etic:al mass orthe c:tv-omium(•l) e-tna.noate
= tnOies x l'l"'ttI.ar m ass
(c) ~yield = ~:~~: x 1009' - 0.00847mol • 376.o szmol- 1
= 70~ ...-": pi~ .,.... f or >SO~ = 3. 19 a V" Allow 3.18
(d) If a iiO"Ned to r ise, a second nitro a:I"'' up
subsVtuted into "the rina V"
~uld b~
( b ) 9-' yia kl =~X 100~
•· · ~ a
(e) The nlti"'t''iu m i on. N o 2• V' - 60~ ......
(f) To 1"9~ 01.ny solu'tion that will c;.ont01.in 50luble iiTipuritMu V" (C) Either some solution of tt'le C~ Ions remained In the
44 (a) The bl u~ soll.ltion '<N'Ould ro ..m a pal e blu~ pl"'ec:l pltate ....-: rou nd· botto.......-d fl ~sk; or soma c.h .-omium(u) ~h~no:~~t:a

• w hic:h dissotvti to
ammonia
~ .a dar k blue solution V" with ex.c;ess

{b) It is a d-.r"k. b luo-p1..wpha ~olid

crysta IS V'
....-; with neQCIIo sn aped
(o)
complex stayed d issol ved in the water V'
(d) c~o,.l-(:~.q) + 1.,. 1-t -(~q) + 6e- -
Cr3-(aq ) -+- e -
Bec.:~.uso
~ ~(aq) .,
2~(~q) + 71-4,0(1) V"

hyd r o a on is producod by t:no ro:lc:'t.ion of :zinc and

..
{c) Amount of hyd •·~d copper-sulfate = ma55/IT'lQI.armas-.. add and pressure mus"'t not. be allowed t.o build up until all
= 6.00 g t l"lo chromium h.:ls boan I"Gduc:ad t:o cr2-......
249.6 grnot-• (f) The d i fferent. l hzands spll"'t 'the d - ort>tt.als of thecr--..
ion to a
- 0 .02AOmol V" diffororrt oxt:an't. .,.-

U nrt 3 and 6: Chemistry Labor"atory Skills

 I ndex

chrom lun'l(u) e th anoate complex preparation 56

A
aceta racy 19. 23. 2 4 colour changes a
actd/base tltrattons 19-20 nntne test 10
odtne/thiOSul fate Utt·a t lons 21
acids
pi-t tttrauons 46- 47 o x1e1auon or a l coh o l s ~~

testing f or 13. 36- 37 1'ed ox uuauons 44

activation energy oxpcrln,cnts 49- 50 tes t s of Ino rganic subs t a n ces 4 0-43
alcohols tests of o rga nt c s ubstan ces 14 - 1 s . 34-37
dehydrauo n o r :>J --.::)2 combu stion tests 14, 34
dlstlns_uts htng rro rn actds ~6-37 conce ntrated su l furic acid test for i n organ i c
halides 11
oxidation to Cllffel"entlal tentary and o ther 14
OXIdatiOn or primary/secondary ~0-3 1 D
tests for OH Q r ou p tn 36 d.ehydra u on o r an a l cohol 3 1-32
aldehydes. tests for 3 1, 35 di splayed formu lae 3!':>
alkenes. tests for 14, 3 4 double salt preparation 28-29
O:lmmo nla addition /excess 42
E
ammonium chloride, h eat test 9 enthalpy c hanQ:e expertment.s 6 , 17 , 22-2~

ammonium sail~. tes t for 10 - 11 ca l c ulatio ns 2 4 -26

8,40
ueous sHveJ"
Arrhentu s equauon
ntua te
49
11 - 12 . 10. 3 4 --.3~ . :>7, 40-4 1
F
experimental m eth o ds 23-24
..
name tes t 9-IO
asplr'ln preparatio n ~!)-0-4

G
B Qraph p lotung 46--47
barium ch l ottde 12. 4 0
acuvauon enerQy 49. .50
c errors In 23-24
ca l cu lations
acuvauon energy 49-.50
H
halide tes t s
entha lpy c h a nge 24-26
concentrated s u l rurtc actd tes t 11
m o lar n1ass 20
u s tnQ: actdtneo sliver nlttate tl- 12. 4 0-41
percentage yie ld 27, 5 1
halog:enoalkanes, tests for 15, 34-35
redox tttratlons 45
h eattng of solids 9
tltratto n .s 19 - 20
hydrated copper(n) I o n s 42
water o f crysta lllsau o n 20
hydrogenc arbonate tests 9, 10
carbonate t ests 9. 10. 41 hydro xide solubility tes t 12- 13
carboxylic actd t est s ~6-.:37
cau ons a. :)9
C=C (alkene) Qroup, tests for 14, 34 Infrare d spcctn:t 16- 17, 37
Chlorine water. addition or 12, 42 tnorganlc naLtdes , tes t rot' 11

76 Edexcel AS/ A2 Ct"'QI'r"''i stry

 Index

I norganic preparations 27
0
chromlun'l(u) ctha n oatc con'lpl ex 56 observation see qua l itative observation
doubl e suit preparation 28- 29 OH s;crot..•P. tests ror 14, 34. 36, 37
Simple salt pn!parauon 27- 28
o r de 1· of r eaction experiment 47- 48
tetraammtnecopper(u) s u trate !S!S o r ganic preparations 29-.30, 51
Inorganic s ubstances s. 39--40 aspi rin 53- 54
tests on 9 - 13, 40-43 dehydration of an alcohol 3 1- 32
todlne/ thfos t.alfate tltratfons 21 -22 murk sch eme 53
Iodoform test .36 measuren,ent or metttng temperatures 52-5.3
methyl 3-nllrobenzoate .54
K
ketones. tests for 3 1. 35 oxidation of prtmal'y/seconaary alcohol 30-31
ktncuc expcrtn,cnts 7. 47- 50 oraantc substances 1~. 33-34
spectra 15-17, 37- 39
L tests for identifying 14 - 16, 3~7
H gand exchanse 42 oxldatton
to differentiate between tentary and other
M a lcohols 14
n,agnes1un1 ana aCid reacuon, acuvauon
energy 13. so. 68-69 primary or secondary alcoh o l 30-31
p
•
n ·u:. rk scheJ'n.es.
Q:l"'aph PIOtttng: 4 6
lnorgantc preparations 55
percentage yteld
pH tests 14, 3 4
27, ~~ ..
klnett c expert ments 48. 49 pH tttrauons 7 , 46-47
observation s 8. 34, 39 potassium Iodide 21. 42
organic preparations 31, 53 potassium manganate(vn) tlt•·atlon 6. 44- 46
salt pl"'epar.::.tton 27, 29 preparations 7 , 27
Utrnuons 19. 45 lnorgo.n l c 27- 29, ss- s6
rna:ss 27.51 organic 29- 32, 5 1- 54
rnass spectra 15 - 16, 37 prln'lary alcohols 14, 30, 37
measu.-e1nent see quanutauve measurement
rnetUng temperatures. methods or Q
quallUHive observau on 5-6. B
rnea.su ring 52- 53
n,elhyl .3-nuroDenzoate preparau on 54
t r'lorgantc substa11ces 8-1~. !>9-44
org:an.l c substances 1!>-17. 33-39
molar mass ca tc uJauons 20
Quantitative measu r e ment 6-7, 17
moles 27. :5 1
e ntha l py cha nge experiments 22-26
N kinetic experhnents 47- 50
nitrate tests 9. 12. 41 titrauons 17-.22. 44 - 47
NMR spectra 38 quostrons and answers 57- 69

U nrt 3 and 6: Chemistry Labor"atory Skills 77

 I ndex

n"'ark schen"'e 19
R
redox tests 42--43 weigh i ng 18
redox tttrations 44-45 T o llens· rea~eru 36

s u
sa l t p r eparation 27- 29 U11tt ~ preparation 27
sccondnry alcohols 14 , 30- 31, 37 lnorQ"anlc 27-29
s i mpl e sa l t prcpun:tUon 27- 28 organ rc .29-32
skeletal forn"'Lilae 33 Un i [ 3 qualitative obser vation 8
!SOdtun'\ hydroxide, addition/excess I n organ ic substances 8 - 13
sodlum thiosulfate and acid reacuon organlc substances 13 - 17
SOl idS Uni t 3 quantitative rneasu rernenl 17
appearance of 40 entha l py c ha1'Q,e experiments 22-26
tests on 9-11 tltratto ns 17-22
solution s Unit 6 preparation s a
nppear~nce of 40 I n organ ic SS-56
tests on 11 - 13 organ ic S l - 54
spcct t·a 15 - 17• .37- 39 Uni t 6 qualitative obscrvuuon
structu ral f ormu l ae 33 tnorgantc s ub~tun ce.s 39-44

•
i'>' 11fate test 12. 40 orsanrc .substances ~3-.:)9
U11lt 6 Quanutauve tneasu1'e1neru 44
..
kinetic experiments 47-50
tertl.;a r y alcohol s 14
pl-l tltratfon s 46- 47
tetraa mm inecopper(u) su lfate preparation 66
redox tttrat i ons 44- 45
tttrauons for A2 6-7
uni versa l I nd icator (UI)
p l ..f ttt ratlons 46- 47
tests 14 , 34, 36
redox titrauons 4 4 - 45
tt t ratlons for AS 6. 17- 18 vv
.acid/base 19- 20 wa t er of ct·yst a l llsatlon calculnt ton 20
errors t o avoid 18-19 water sol ublllty tes ts 14, .34
todrne/Lhlosulfate 21-22 weighing- 18

78 Ede><:Cel AS/A2 ChEHY'IIstry

c 1 2 Group 3 4 6
,..
:>
5 7 0

"'~ P~1oo
1
~
H
4.0

P.'
()
h)'d«Jg!f'l
1 .....
He

"'"'3"
2

-
6.9 9.0 The periodic table 10.8 12.0 14 0 16-0 19.0 20.2
~·
I»
8'
2 Ll
'"""
3
Be
ber,llh1m
4 Key: R~attve atomic mass
B
'""' """"
5 6
c N
7
0
..,.., ....,
8
F
9
.. Ne
......
10
:a.o Atomic symbol
!!!: 3 Na
so:llllln
24.3

...,...,....,
Mg ""' number
Atomic (proton)
27.0
AI
:.h.n'f!Un
28.1

....,.
Si
31.0
p
ph:Jsphorus
32.1
s
......
355
Cl
chlom~t
39.9
Ar
.....
II 12 13 14 15 16 17 18
"'
4
39.1
K
..........
19
855
40.1
Ca
a klwn
20
87.6
45.0
Sc
tcillndtum
21
88.9
47.9
Ti
tltllnl.lm
22
9 1.2
50.9
v
..........
23
92.9
Sl.O
Cr
t'-"llm
24
95.9
549

-..-
Mn
25
(98]
55.8
Fe
·~
26
101.1
58.9
Co
""""
27 '"'"
102.9
28
58.7
Ni

106A
635
Cu
~-
29
107.9
6SA
Zn
""'
30
112A
Ga
.. -
69.7

31
114.8
72.6
Ge
~IWiillllll ..

32
l lt\.7
749
As
·-·33
121.8
79.0

.......
Se
34
127.6
-
79.9
Br
35
126.9
83.8
Kr
.,,.~

36
131.3 L-

• 5
N-Rb
37
132.9
Sr
wontklm
38
1373
y
,.....,
39
138.9
Zr
'"""'""
40
178.5
Nb
niobium
41
18o.9
Mo
--~
42
183.8
Tc
43
186.2
Ru
tedln!tll.lm ruthenium
4d
190.2
Rh
1hochu,.
45
192.2
Pd
P"'_.lllm
46
195.1
Ag
··-
47
197.0
Cd
ad.....,

20M
48 ·-In
49
2044
Sn

207.2
Sb Te
•so• .........,
51 52
209.0
~klfklm

(209]
""~
53
I

(210]
Xe
-·
54
(222]
II
r-

Cs Ta w Re lr Pt Hg n Bi Po Rn
6
"""m
55
...Ba... La,
S6
....M ~
Hf
..........
72
WUII.Im
73
tung~n
74 '""'""
75
Os
(11;1!1111111

76
• •clt.m
77
.........
78
Au
gdd
79
~W'1

80
thlll• m
81
....Pb
82
bhn•ttl
83
pobnll~
84
At
t i. .. .

85 """'
86
(223] (226] (227] (261] (262] (266] (264] (277] (268] (271] (272]
Fr Ra Ac Sg Bh Elements with atomic numbers 112-116 have been
Db
......Hs. Mt Ds Rg
"-
Rf
7
-·~
87 88
actinium
89
rthlbiAI•
104
...,..
105 -~""
106 """''""
107 108
..en-lum <bn.d!ll
109 110 ·- ·
111
reported but not fully authenticated

-
140.1 140.9 144.2 144.9 ISOA 152.0 157.2 158.9 162.5 1649 1673 168.9 173.0 175.0
Dy
Ce
""'m
58
Pr
59
....Nd,...
60
~
Pm
J:lOmethlu
61
Sm
D -ot.m
61
Eu
«Jtopillm
63
...,.Gd...... .....
64
Tb
65
. Ho
Y'Ff'"IUm holmlllm
66 67
-~~
Er
68
..Tm
. . ...
69
Yb
"'""~
70
lu
II.Cetllm
71

232
Th
........
90
(23 1]
Pa
"'"""''
91
238. 1

...,u...
92
Np
(237]

ft!l'(unliM
93
(242]

94
Pu
~··"'
(243]
Am
3olll!fi( 1Utn

95
f247]
Cm
(UIIIJM
96
(245]
Bk
belk.fflllr'l
97
[251]
Cf
(254]
Es
CellfotiiiUrl tii'IStf:taii,M

98 99
1253]
Fm
""'""
100
(256]
Md .,_,.,
101
No lr
(254]

.........,
102
.(257]

103

;2J